CN108864801A - A kind of preparation method of salt tolerant higher suspension thickener for coating - Google Patents
A kind of preparation method of salt tolerant higher suspension thickener for coating Download PDFInfo
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- CN108864801A CN108864801A CN201810827908.8A CN201810827908A CN108864801A CN 108864801 A CN108864801 A CN 108864801A CN 201810827908 A CN201810827908 A CN 201810827908A CN 108864801 A CN108864801 A CN 108864801A
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- 239000002562 thickening agent Substances 0.000 title claims abstract description 54
- 238000000576 coating method Methods 0.000 title claims abstract description 49
- 239000011248 coating agent Substances 0.000 title claims abstract description 48
- 239000000725 suspension Substances 0.000 title claims abstract description 47
- 150000003839 salts Chemical class 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 32
- 239000003292 glue Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920002678 cellulose Polymers 0.000 claims abstract description 21
- 239000001913 cellulose Substances 0.000 claims abstract description 21
- 229920000297 Rayon Polymers 0.000 claims abstract description 18
- 150000001768 cations Chemical group 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 90
- 235000008708 Morus alba Nutrition 0.000 claims description 46
- 240000000249 Morus alba Species 0.000 claims description 46
- 239000000706 filtrate Substances 0.000 claims description 41
- 238000001914 filtration Methods 0.000 claims description 32
- 239000002893 slag Substances 0.000 claims description 27
- 239000007787 solid Substances 0.000 claims description 27
- 238000009835 boiling Methods 0.000 claims description 26
- 239000007795 chemical reaction product Substances 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 125000002091 cationic group Chemical group 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 19
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 19
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 19
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000012043 crude product Substances 0.000 claims description 14
- 210000003097 mucus Anatomy 0.000 claims description 14
- 238000009423 ventilation Methods 0.000 claims description 14
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 claims description 13
- 239000013049 sediment Substances 0.000 claims description 13
- 239000012991 xanthate Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 11
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 239000000908 ammonium hydroxide Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 9
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000460 chlorine Substances 0.000 claims description 8
- 229910052801 chlorine Inorganic materials 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 7
- GBCKRQRXNXQQPW-UHFFFAOYSA-N n,n-dimethylprop-2-en-1-amine Chemical compound CN(C)CC=C GBCKRQRXNXQQPW-UHFFFAOYSA-N 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 230000004044 response Effects 0.000 claims description 6
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 6
- 230000003519 ventilatory effect Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 3
- ZCHPKWUIAASXPV-UHFFFAOYSA-N acetic acid;methanol Chemical compound OC.CC(O)=O ZCHPKWUIAASXPV-UHFFFAOYSA-N 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims description 2
- 238000000703 high-speed centrifugation Methods 0.000 claims description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 2
- 239000003973 paint Substances 0.000 abstract description 15
- 239000000049 pigment Substances 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 7
- 230000003993 interaction Effects 0.000 abstract description 5
- 229920002521 macromolecule Polymers 0.000 abstract description 5
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 229920003086 cellulose ether Polymers 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000004804 winding Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 37
- 239000007789 gas Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 102000004190 Enzymes Human genes 0.000 description 5
- 108090000790 Enzymes Proteins 0.000 description 5
- 230000008719 thickening Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000007665 sagging Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 230000015784 hyperosmotic salinity response Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/43—Thickening agents
- C09D7/44—Combinations of two or more thickening agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/193—Mixed ethers, i.e. ethers with two or more different etherifying groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B9/00—Cellulose xanthate; Viscose
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention belongs to thickener preparation technical fields, and in particular to a kind of preparation method of salt tolerant higher suspension thickener for coating.Amphoteric cellulose ether in the present invention can effectively weaken and prevent in water paint free water molecule in coating particles and surface of pigments aquation, improve the consistency of coating, prevent pigment sedimentation, electrostatic force is only electrostatic attraction in strand in thickener for coating, polymer molecule is caused to shrink, hydrodynamic volume reduces, thickening agent carrier used is cellulose viscose glue, it can be hydrated with hydrone by hydrogen bond rapidly, and pass through the winding between fiber molecule, improve the standing viscosity of water paint, a large amount of cation group has preferable repulsive interaction to metal cation, it can avoid heavy metal ion in the pigment of water paint simultaneously and destroy macromolecule surface moisture film, to make thickener that there is good salt resistant character, it has a extensive future.
Description
Technical field
The invention belongs to thickener preparation technical fields, and in particular to a kind of preparation of salt tolerant higher suspension thickener for coating
Method.
Background technique
Modern architecture, construction, house ornamentation all be unable to do without coating, paint.The use of coating is not only to decorate, can also be effectively
Protection basis material, extend building, the service life of equipment etc..Water paint is a kind of low pollution, saves the energy, resource-saving
Coating.With the reinforcement of people's environmental consciousness, water paint is increasingly subject to the attention of people, and Related product is widely studied
And exploitation.Water paint is usually by the dispersion of the emulsion particle of resin, pigment suspension particle, by interparticle mutual
Active force and formed.The viscosity of coating is the characterization of these particle interaction power, and still, these active forces are weaker, thickening
The effect of agent is to increase interparticle interaction, forms network structure.
Thickener is a kind of auxiliary rheological agents.Thickener is added in coating can increase the viscosity of coating, and pigment is made slowly to sink
It forms sediment, to be easy to stir evenly, and then guarantees coating storage stability.The addition of thickener can make coating have centainly thick
Degree and thixotropy brush laborsaving, and drip and sagging when can reduce application in construction, guarantee the appearance and matter of dope layer
Amount.For water paint lower for viscosity, it is very important an analog assistant.
Ideal coating is preferably during storage, or can form solid immediately after homogenous application, thus will not
The separation of pigment or color occurs, but it is actually required to be suitable for applying the liquid of operation.Then pigment is just produced
The problems such as sedimentation separation, drying property, levelability, sagging.Customary thickeners have:Inorganic thickening agent, modified cellulose, polyacrylic acid
The polyurethane thickener of ester and association type.The macromolecules such as cellulose thickener, agent for polyacrylic acid thickening and polyurethane thickener
Thickener at paste property and in terms of performance it is prominent, have a wide range of applications.But they are high in the prevalence of price,
The defects of electrolyte-resistant ability is poor.Inorganic thickening agent also has good thickening capabilities, because of its tool cheap and in use
Have the advantages that thixotropic index is big, sag resistance can good, pH wide adaptation range, be widely used.It should be pointed out that inorganic thickening agent
Thickening capabilities are much smaller than high molecular polymer thickener, therefore are limited use scope.
The thickener of building trade coating is many kinds of at present, but exist mostly suspension, anti-settling property, stability and
The disadvantage of levelability difference, can not accomplish the effect that can thicken in different pH value coating, and it is in anti-layering, resist sagging
The performance of aspect is also poor, so that coating is affected in production, storage, construction, film forming procedure.Therefore, thickener is improved
Anti-settling property seem extremely important.
Therefore, a kind of anti-settling property, levelability and the good thickener for coating of stability are prepared, there is important theory
Meaning and application value.
Summary of the invention
Present invention mainly solves the technical issues of, traditional thickener for current water paint is mainly common organic water
Soluble macromolecular material, they cannot weaken the hydration of emulsion particle in water paint, lead to the salt resistant character of thickener
Difference, the defect of suspension stability difference provide a kind of preparation method of salt tolerant higher suspension thickener for coating.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of salt tolerant higher suspension thickener for coating, it is characterised in that specifically preparation step is:
(1)150~160mL epoxychloropropane is added into the three-necked flask with blender and snorkel, three-necked flask is set
In ice-water bath, front three amine gas is led into three-necked flask, starts blender, is stirred with the revolving speed of 200~250r/min, ventilation
It is separated by filtration to obtain white solid product after reaction, is put into and sets in vacuum oven, be dried to obtain cationic etherifying agent;
(2)30~35g hydroxyethyl cellulose, 120~140mL sodium hydroxide solution and 8~10g cation are added into reactor
Etherifying agent is stirred to react, and obtains reaction product, is neutralized reaction product with hydrochloric acid, is obtained suspension, and suspension is placed in high speed
Centrifugal treating in centrifuge removes upper liquid, collects lower sediment thing, sediment is placed in oven and dried, cation is obtained
Hydroxyethyl cellulose;
(3)Mulberry skin machinery is blended, removal filtrate obtains mulberry skin slag, and 80~120g mulberry skin slag is placed in a beaker, and 4~5g is added
Degummase and 200~300mL distilled water, enzymatic hydrolysis, filtering removal filtrate obtain enzymatic hydrolysis fiber, clean enzymatic hydrolysis with sodium hydroxide solution
Fiber obtains mulberry skin and removes glue fiber, goes glue fiber to be put into the four-hole boiling flask with blender and dropping funel mulberry skin obtained
In, 400~450mL ammonium hydroxide is added into four-hole boiling flask, 15~18mL is added dropwise into four-hole boiling flask with dropping funel for heat temperature raising
Carbon disulfide is stirred to react, and obtains reaction product;
(4)30~35min, filtering is mixed in above-mentioned reaction product and 400~500mL Adlerika, removal filtrate obtains
To filter residue, filter residue being washed with dehydrated alcohol, yellow solid is obtained, yellow solid is placed in baking oven, heat temperature raising is dry,
The xanthate of mulberry skin slag is obtained, 100~120mL sodium hydroxide solution is added into the xanthate of mulberry skin slag, obtains fiber
Plain viscose;
(5)40~45mL dimethylallylamine is added into the four-hole boiling flask with condensing unit, heat temperature raising is burnt to four mouthfuls
5~7g monoxone and 60~70mL sodium hydroxide solution are added in bottle, are stirred with magnetic stirring apparatus with the revolving speed of 300~400r/min
It being transferred in distilling flask after mixing reaction, heat temperature raising, distillation obtains the suspension containing white crystal, continuously add 100~
110mL dehydrated alcohol is centrifugally separating to obtain the light yellow mucus in upper layer;
(6)The above-mentioned light yellow mucus of 40~50mL and 80~100mL deionization are added into the three-necked flask equipped with condensing unit
Water, then chlorine is passed through into three-necked flask, the pH of reaction system in three-necked flask, heat temperature raising are controlled, distillation continues to three mouthfuls
70~80mL dehydrated alcohol is added in flask, is separated by filtration to obtain thick filtrate;
(7)30~35g cationic hydroxyethyl cellulose is added into thick filtrate, is stirred to react to obtain solid crude product, it will
Solid crude product and cellulose viscose be put into acetic acid methanol solution impregnate 40~50min, be separated by filtration removal filtrate obtain it is wet
Wet glue is put into vacuum oven by glue, dry, is ground up, sieved to obtain salt tolerant higher suspension thickener for coating.
Step(1)The Ventilation Rate is 40~50mL/min, and the ventilatory response time is 4~5h, and vacuum oven is set
Determining temperature is 70~80 DEG C, and drying time is 6~7h.
Step(2)The mass fraction of the sodium hydroxide solution is 15%, and being stirred to react the time is 1~2h, the matter of hydrochloric acid
Measuring score is 20%, and high speed centrifugation revolving speed is 2000~3000r/min, and the centrifugal treating time is 8~10min, baking oven set temperature
It is 60~70 DEG C, drying time is 4~5h.
Step(3)The enzymolysis time is 2~3h, and the mass fraction of sodium hydroxide solution is 30%, the quality point of ammonium hydroxide
Number be 20%, heat temperature raising temperature be 60~65 DEG C, dropping funel drop rate be 3~5mL/min, be stirred to react the time be 2~
3h。
Step(4)The mass fraction of the Adlerika is 25%, and heat temperature raising temperature is 50~55 DEG C, when dry
Between be 2~3h, the mass fraction of sodium hydroxide solution is 20%.
Step(5)The heat temperature raising temperature is 55~60 DEG C, and the mass fraction of sodium hydroxide solution is 20%, stirring
Reaction time is 20~30min, and heat temperature raising temperature is 70~80 DEG C, and distillation time is 1.5~2.0h.
Step(6)The Ventilation Rate is 30~35mL/min, leads to the pH of reaction system in chlorine control three-necked flask
It is 6~7, heat temperature raising temperature is 80~90 DEG C, and distillation time is 2~3h.
Step(7)The time that is stirred to react is 30~40min, and the mass fraction of the methanol solution of acetic acid is 20%, very
Empty drying box set temperature is 70~80 DEG C, and drying time is 10~12h, and be sieved specification is 200 mesh.
The beneficial effects of the invention are as follows:
(1)The present invention is passed through front three amine gas in low temperature into epoxychloropropane, is stirred to react to obtain reaction product, passes through
It filters, be dried to obtain cationic etherifying agent, after being etherified hydroxyethyl cellulose under alkaline condition with cationic etherifying agent, by centrifugation
It separates, be dried to obtain cationic hydroxyethyl cellulose, mulberry skin machinery is blended to obtain mulberry skin slag, enzymolysis method for degumming digests fiber, uses
Caustic dip digests fiber, obtains mulberry skin and removes glue fiber, goes to add ammonium hydroxide in glue fiber to mulberry skin obtained, with carbon disulfide yellow
Xanthate is prepared, cellulose viscose is obtained, dimethylallylamine, monoxone, sodium hydroxide solution are mixed, are stirred to react
Light yellow liquid is obtained, by distilling, being obtained by filtration light yellow mucus, heats distillation after chlorine is passed through into light yellow mucus,
Dehydrated alcohol is added, thick filtrate filtrate is obtained by filtration, thick filtrate and cationic hydroxyethyl cellulose are stirred anti-
It answers, obtains solid crude product, solid crude product is mixed into methanol solution immersion treatment, mistake through peracetic acid with cellulose viscose glue
It filters, be dried to obtain salt tolerant higher suspension thickener for coating, the present invention first under alkaline condition, utilizes hydroxyethyl cellulose strand
On active hydroxyl groups and epoxychloropropane etherification reaction occur obtain cationic hydroxyethyl cellulose ethers, then be prepared sticky
Shape filtrate is a kind of anionic amino salt, thus thick filtrate can be used to load cationic hydroxyethyl cellulose ethers anionic
Salt tolerant higher suspension thickener for coating is obtained in cellulose viscose glue, thickener of the invention is fine by the load both sexes of cellulose viscose glue
It ties up plain ether to be prepared, amphoteric cellulose ether can effectively weaken and prevent in water paint free water molecule in coating particles
With surface of pigments aquation, meanwhile, the solvated layer that a large amount of anionic groups have can improve the coagulation stability of system again, in this way
Amphoteric cellulose ether can be improved the aquation dispersibility of particle in water paint, improve the resistance of motion of hydrone, suspend
Stability is improved, and is improved the consistency of coating, is prevented pigment sedimentation;
(2)The number of anions and canons group is roughly equal in thickener for coating of the invention, electrostatic force in strand
Only electrostatic attraction, in aqueous solution, this electrostatic attraction effect make to generate in coating in polymeric groups and in strand
Association causes polymer molecule to shrink, and hydrodynamic volume reduces, and solution viscosity becomes smaller, and furthermore thickener used carries
Body is cellulose viscose glue, it can be hydrated with hydrone by hydrogen bond rapidly, forms continuous homogeneous system with water, and pass through fibre
Intermolecular winding is tieed up, the standing viscosity of water paint is improved, prevents pigment sedimentation, due in molecular radical and in strand
Association is shielded by small molecule electrolyte, so that the interaction ability of macromolecule and solvent enhances, molecular conformation is gradually
Become to unfold, solution viscosity increases, to show apparent anti-polyelectrolyte solution behavior, Water Content in Water-reducible Paints compared with
Still biggish consistency can be kept when high, weaken the osmosis of salting liquid, and a large amount of cation group to metal sun from
Son also has preferable repulsive interaction, while heavy metal ion destroys macromolecule surface moisture film in the pigment of avoidable water paint,
It is gathered in the macromolecule surface with anion, to make thickener that there is good salt resistant character, is had a extensive future.
Specific embodiment
150~160mL epoxychloropropane is added into the three-necked flask with blender and snorkel, three-necked flask is set
In ice-water bath, front three amine gas is led to the Ventilation Rate of 40~50mL/min into three-necked flask, starts blender, with 200
The revolving speed of~250r/min stirs, and is separated by filtration to obtain white solid product after 4~5h of ventilatory response, and being put into set temperature is 70
In~80 DEG C of vacuum oven, dry 6~7h obtains cationic etherifying agent;It is fine that 30~35g ethoxy is added into reactor
Dimension element, the sodium hydroxide solution and 8~10g cationic etherifying agent that 120~140mL mass fraction is 15%, are stirred to react 1~2h,
Reaction product is obtained, reaction product is neutralized with the hydrochloric acid that mass fraction is 20%, obtains suspension, suspension is placed in high speed
With revolving speed 8~10min of centrifugal treating of 2000~3000r/min in centrifuge, upper liquid is removed, collects lower sediment thing, it will
Sediment is put into dry 4~5h in the baking oven that set temperature is 60~70 DEG C, obtains cationic hydroxyethyl cellulose;By mulberry skin machine
Tool blends, and removal filtrate obtains mulberry skin slag, and 80~120g mulberry skin slag is placed in a beaker, be added 4~5g degummase and 200~
300mL distilled water, digests 2~3h, and filtering removal filtrate obtains enzymatic hydrolysis fiber, the sodium hydroxide solution for being 30% with mass fraction
Cleaning of enzyme solution fiber obtains mulberry skin and removes glue fiber, goes glue fiber to be put into blender and dropping funel mulberry skin obtained
In four-hole boiling flask, the ammonium hydroxide that 400~450mL mass fraction is 20% is added into four-hole boiling flask, is heated to 60~65 DEG C,
15~18mL carbon disulfide is added dropwise into four-hole boiling flask with the drop rate of 3~5mL/min with dropping funel, it is stirred to react 2~
3h obtains reaction product;The Adlerika that above-mentioned reaction product and 400~500mL mass fraction are 25% is mixed 30
~35min, filtering, removal filtrate obtain filter residue, filter residue are washed with dehydrated alcohol, yellow solid is obtained, yellow solid is set
In baking oven, 50~55 DEG C are heated to, dry 2~3h obtains the xanthate of mulberry skin slag, to the xanthate of mulberry skin slag
The middle sodium hydroxide solution that 100~120mL mass fraction is added and is 20%, obtains cellulose viscose;To four with condensing unit
40~45mL dimethylallylamine is added in mouth flask, is heated to 55~60 DEG C, 5~7g chlorine is added into four-hole boiling flask
The sodium hydroxide solution that acetic acid and 60~70mL mass fraction are 20%, is stirred with magnetic stirring apparatus with the revolving speed of 300~400r/min
It is transferred in distilling flask after mixing 20~30min of reaction, is heated to 70~80 DEG C, distill 1.5~2.0h, obtained containing white
The suspension of crystal continuously adds 100~110mL dehydrated alcohol, is centrifugally separating to obtain the light yellow mucus in upper layer;To equipped with condensation
The above-mentioned light yellow mucus of 40~50mL and 80~100mL deionized water are added in the three-necked flask of device, then into three-necked flask
It is passed through chlorine with the Ventilation Rate of 30~35mL/min, the pH for controlling reaction system in three-necked flask is 6~7, is heated to
80~90 DEG C, 2~3h is distilled, continues that 70~80mL dehydrated alcohol is added to three-necked flask, is separated by filtration to obtain thick filtrate;
30~35g cationic hydroxyethyl cellulose is added into thick filtrate, is stirred to react 30~40min and obtains solid crude product,
Solid crude product and cellulose viscose are put into the methanol solution that mass fraction is 20% acetic acid and impregnate 40~50min, is separated by filtration
Removal filtrate obtains wet glue, wet glue is put into the vacuum oven that set temperature is 70~80 DEG C, dry 10~12h, grinding
It crosses 200 meshes and obtains salt tolerant higher suspension thickener for coating.
Example 1
150mL epoxychloropropane is added into the three-necked flask with blender and snorkel, three-necked flask is placed in ice-water bath
In, front three amine gas is led to the Ventilation Rate of 40mL/min into three-necked flask, starts blender, is stirred with the revolving speed of 200r/min
It mixes, is separated by filtration to obtain white solid product after ventilatory response 4h, be put into the vacuum oven that set temperature is 70 DEG C, it is dry
6h obtains cationic etherifying agent;30g hydroxyethyl cellulose is added into reactor, the hydroxide that 120mL mass fraction is 15%
Sodium solution and 8g cationic etherifying agent, are stirred to react 1h, obtain reaction product, are produced reaction with the hydrochloric acid that mass fraction is 20%
Object neutralizes, and obtains suspension, suspension is placed in the revolving speed centrifugal treating 8min in supercentrifuge with 2000r/min, removes
Upper liquid collects lower sediment thing, and sediment is put into dry 4h in the baking oven that set temperature is 60 DEG C, obtains cationic hydroxyl second
Base cellulose;Mulberry skin machinery is blended, removal filtrate obtains mulberry skin slag, and 80g mulberry skin slag is placed in a beaker, and 4 degummases are added
With 200mL distilled water, 2h is digested, filtering removal filtrate obtains enzymatic hydrolysis fiber, and the sodium hydroxide solution for being 30% with mass fraction is clear
Wash enzymatic hydrolysis fiber, obtain mulberry skin and remove glue fiber, by mulberry skin obtained go glue fiber be put into blender and dropping funel four
In mouthful flask, the ammonium hydroxide that 400mL mass fraction is 20% is added into four-hole boiling flask, is heated to 60 DEG C, with dropping funel with
15mL carbon disulfide is added dropwise into four-hole boiling flask for the drop rate of 3mL/min, is stirred to react 2h, obtains reaction product;It will be above-mentioned
30min, filtering is mixed in the Adlerika that reaction product and 400mL mass fraction are 25%, and removal filtrate obtains filter residue,
Filter residue is washed with dehydrated alcohol, yellow solid is obtained, yellow solid is placed in baking oven, is heated to 50 DEG C, dry 2h,
The xanthate of mulberry skin slag is obtained, it is molten that the sodium hydroxide that 100mL mass fraction is 20% is added into the xanthate of mulberry skin slag
Liquid obtains cellulose viscose;40mL dimethylallylamine is added into the four-hole boiling flask with condensing unit, is heated to
55 DEG C, the sodium hydroxide solution that 5g monoxone and 60mL mass fraction are 20% is added into four-hole boiling flask, with magnetic stirring apparatus with
The revolving speed of 300r/min is transferred in distilling flask after being stirred to react 20min, is heated to 70 DEG C, is distilled 1.5h, is contained
The suspension of white crystal continuously adds 100mL dehydrated alcohol, is centrifugally separating to obtain the light yellow mucus in upper layer;To equipped with condensation
The above-mentioned light yellow mucus of 40mL and 80mL deionized water are added in the three-necked flask of device, then into three-necked flask with 30mL/min
Ventilation Rate be passed through chlorine, the pH for controlling reaction system in three-necked flask is 6, is heated to 80 DEG C, distills 2h, continue to
70mL dehydrated alcohol is added in three-necked flask, is separated by filtration to obtain thick filtrate;30g cation hydroxyl is added into thick filtrate
Ethyl cellulose is stirred to react 30min and obtains solid crude product, and solid crude product and cellulose viscose are put into mass fraction and are
The methanol solution of 20% acetic acid impregnates 40min, is separated by filtration removal filtrate and obtains wet glue, and it is 70 DEG C that wet glue, which is put into set temperature,
Vacuum oven in, dry 10h, ground 200 mesh obtains salt tolerant higher suspension thickener for coating.
Example 2
155mL epoxychloropropane is added into the three-necked flask with blender and snorkel, three-necked flask is placed in ice-water bath
In, front three amine gas is led to the Ventilation Rate of 45mL/min into three-necked flask, starts blender, is stirred with the revolving speed of 225r/min
It mixes, is separated by filtration to obtain white solid product after ventilatory response 4h, be put into the vacuum oven that set temperature is 75 DEG C, it is dry
6h obtains cationic etherifying agent;33g hydroxyethyl cellulose is added into reactor, the hydroxide that 130mL mass fraction is 15%
Sodium solution and 9g cationic etherifying agent, are stirred to react 1h, obtain reaction product, are produced reaction with the hydrochloric acid that mass fraction is 20%
Object neutralizes, and obtains suspension, suspension is placed in the revolving speed centrifugal treating 9min in supercentrifuge with 2500r/min, removes
Upper liquid collects lower sediment thing, and sediment is put into dry 4h in the baking oven that set temperature is 65 DEG C, obtains cationic hydroxyl second
Base cellulose;Mulberry skin machinery is blended, removal filtrate obtains mulberry skin slag, and 100g mulberry skin slag is placed in a beaker, and 4g degumming is added
Enzyme and 250mL distilled water, digest 2h, and filtering removal filtrate obtains enzymatic hydrolysis fiber, the sodium hydroxide solution for being 30% with mass fraction
Cleaning of enzyme solution fiber obtains mulberry skin and removes glue fiber, goes glue fiber to be put into blender and dropping funel mulberry skin obtained
In four-hole boiling flask, the ammonium hydroxide that 425mL mass fraction is 20% is added into four-hole boiling flask, is heated to 63 DEG C, uses dropping funel
17mL carbon disulfide is added dropwise into four-hole boiling flask with the drop rate of 4mL/min, is stirred to react 2h, obtains reaction product;It will be upper
It states reaction product and 450mL mass fraction and 33min, filtering is mixed for 25% Adlerika, removal filtrate is filtered
Filter residue is washed with dehydrated alcohol, obtains yellow solid, yellow solid is placed in baking oven by slag, is heated to 53 DEG C, drying
2h obtains the xanthate of mulberry skin slag, and the sodium hydroxide that 110mL mass fraction is 20% is added into the xanthate of mulberry skin slag
Solution obtains cellulose viscose;43mL dimethylallylamine, heat temperature raising are added into the four-hole boiling flask with condensing unit
To 53 DEG C, the sodium hydroxide solution that 6g monoxone and 65mL mass fraction are 20% is added into four-hole boiling flask, uses magnetic stirring apparatus
It is transferred in distilling flask after being stirred to react 25min with the revolving speed of 350r/min, is heated to 75 DEG C, distilled 1.7h, obtain
Suspension containing white crystal continuously adds 105mL dehydrated alcohol, is centrifugally separating to obtain the light yellow mucus in upper layer;To equipped with cold
The above-mentioned light yellow mucus of 45mL and 90mL deionized water are added in the three-necked flask of solidifying device, then into three-necked flask with 33mL/
The Ventilation Rate of min is passed through chlorine, and the pH for controlling reaction system in three-necked flask is 6, is heated to 85 DEG C, distills 2h, after
Continue to three-necked flask and 75mL dehydrated alcohol is added, is separated by filtration to obtain thick filtrate;Into thick filtrate be added 33g sun from
Sub- hydroxyethyl cellulose is stirred to react 35min and obtains solid crude product, and solid crude product and cellulose viscose are put into quality point
Number is that the methanol solution of 20% acetic acid impregnates 45min, is separated by filtration removal filtrate and obtains wet glue, wet glue, which is put into set temperature, is
In 75 DEG C of vacuum oven, dry 11h, ground 200 mesh obtains salt tolerant higher suspension thickener for coating.
Example 3
160mL epoxychloropropane is added into the three-necked flask with blender and snorkel, three-necked flask is placed in ice-water bath
In, front three amine gas is led to the Ventilation Rate of 50mL/min into three-necked flask, starts blender, is stirred with the revolving speed of 250r/min
It mixes, is separated by filtration to obtain white solid product after ventilatory response 5h, be put into the vacuum oven that set temperature is 80 DEG C, it is dry
7h obtains cationic etherifying agent;35g hydroxyethyl cellulose is added into reactor, the hydroxide that 140mL mass fraction is 15%
Sodium solution and 10g cationic etherifying agent, are stirred to react 2h, obtain reaction product, are produced reaction with the hydrochloric acid that mass fraction is 20%
Object neutralizes, and obtains suspension, suspension is placed in the revolving speed centrifugal treating 10min in supercentrifuge with 3000r/min, removes
Upper liquid collects lower sediment thing, and sediment is put into dry 5h in the baking oven that set temperature is 70 DEG C, obtains cationic hydroxyl second
Base cellulose;Mulberry skin machinery is blended, removal filtrate obtains mulberry skin slag, and 120g mulberry skin slag is placed in a beaker, and 5g degumming is added
Enzyme and 300mL distilled water, digest 3h, and filtering removal filtrate obtains enzymatic hydrolysis fiber, the sodium hydroxide solution for being 30% with mass fraction
Cleaning of enzyme solution fiber obtains mulberry skin and removes glue fiber, goes glue fiber to be put into blender and dropping funel mulberry skin obtained
In four-hole boiling flask, the ammonium hydroxide that 450mL mass fraction is 20% is added into four-hole boiling flask, is heated to 65 DEG C, uses dropping funel
18mL carbon disulfide is added dropwise into four-hole boiling flask with the drop rate of 5mL/min, is stirred to react 3h, obtains reaction product;It will be upper
It states reaction product and 500mL mass fraction and 35min, filtering is mixed for 25% Adlerika, removal filtrate is filtered
Filter residue is washed with dehydrated alcohol, obtains yellow solid, yellow solid is placed in baking oven by slag, is heated to 55 DEG C, drying
3h obtains the xanthate of mulberry skin slag, and the sodium hydroxide that 120mL mass fraction is 20% is added into the xanthate of mulberry skin slag
Solution obtains cellulose viscose;45mL dimethylallylamine, heat temperature raising are added into the four-hole boiling flask with condensing unit
To 60 DEG C, the sodium hydroxide solution that 7g monoxone and 70mL mass fraction are 20% is added into four-hole boiling flask, uses magnetic stirring apparatus
It is transferred in distilling flask after being stirred to react 30min with the revolving speed of 400r/min, is heated to 80 DEG C, distilled 2.0h, obtain
Suspension containing white crystal continuously adds 110mL dehydrated alcohol, is centrifugally separating to obtain the light yellow mucus in upper layer;To equipped with cold
The above-mentioned light yellow mucus of 50mL and 100mL deionized water are added in the three-necked flask of solidifying device, then into three-necked flask with 35mL/
The Ventilation Rate of min is passed through chlorine, and the pH for controlling reaction system in three-necked flask is 7, is heated to 90 DEG C, distills 3h, after
Continue to three-necked flask and 80mL dehydrated alcohol is added, is separated by filtration to obtain thick filtrate;Into thick filtrate be added 35g sun from
Sub- hydroxyethyl cellulose is stirred to react 40min and obtains solid crude product, and solid crude product and cellulose viscose are put into quality point
Number is that the methanol solution of 20% acetic acid impregnates 50min, is separated by filtration removal filtrate and obtains wet glue, wet glue, which is put into set temperature, is
In 80 DEG C of vacuum oven, dry 12h, ground 200 mesh obtains salt tolerant higher suspension thickener for coating.
The thickener for coating that comparative example is produced with Guangzhou company is as a comparison case to salt tolerant produced by the present invention
Thickener for coating in higher suspension thickener for coating and comparative example is detected, and testing result is as shown in table 1:
Thickener for coating in salt tolerant higher suspension thickener for coating produced by the present invention and comparative example is applied respectively in water
Test sample is made in property formulation for coating material.
Viscosimetric analysis
It is tested using rotary viscosimeter instrument.
Salt tolerance test
First test the viscosity of above-mentioned test sample.Then, 5% sal glauberi is added in the sample respectively, it is right to continue to measure its
The viscosity number answered.
Suspension stability test
Above-mentioned test sample is placed in and stands 3 months at room temperature, observes the appearance of a sample.
1 performance measurement result of table
According to data in table 1 it is found that salt tolerant higher suspension thickener for coating produced by the present invention, have good thickening capabilities,
Sag resistance energy and suspending stabilized performance, and salt tolerance is strong, pH wide adaptation range, manufacture craft is simple, and cost is relatively low, has wide
Wealthy prospect of the application.
Claims (8)
1. a kind of preparation method of salt tolerant higher suspension thickener for coating, it is characterised in that specifically preparation step is:
(1)150~160mL epoxychloropropane is added into the three-necked flask with blender and snorkel, three-necked flask is set
In ice-water bath, front three amine gas is led into three-necked flask, starts blender, is stirred with the revolving speed of 200~250r/min, ventilation
It is separated by filtration to obtain white solid product after reaction, is put into and sets in vacuum oven, be dried to obtain cationic etherifying agent;
(2)30~35g hydroxyethyl cellulose, 120~140mL sodium hydroxide solution and 8~10g cation are added into reactor
Etherifying agent is stirred to react, and obtains reaction product, is neutralized reaction product with hydrochloric acid, is obtained suspension, and suspension is placed in high speed
Centrifugal treating in centrifuge removes upper liquid, collects lower sediment thing, sediment is placed in oven and dried, cation is obtained
Hydroxyethyl cellulose;
(3)Mulberry skin machinery is blended, removal filtrate obtains mulberry skin slag, and 80~120g mulberry skin slag is placed in a beaker, and 4~5g is added
Degummase and 200~300mL distilled water, enzymatic hydrolysis, filtering removal filtrate obtain enzymatic hydrolysis fiber, clean enzymatic hydrolysis with sodium hydroxide solution
Fiber obtains mulberry skin and removes glue fiber, goes glue fiber to be put into the four-hole boiling flask with blender and dropping funel mulberry skin obtained
In, 400~450mL ammonium hydroxide is added into four-hole boiling flask, 15~18mL is added dropwise into four-hole boiling flask with dropping funel for heat temperature raising
Carbon disulfide is stirred to react, and obtains reaction product;
(4)30~35min, filtering is mixed in above-mentioned reaction product and 400~500mL Adlerika, removal filtrate obtains
To filter residue, filter residue being washed with dehydrated alcohol, yellow solid is obtained, yellow solid is placed in baking oven, heat temperature raising is dry,
The xanthate of mulberry skin slag is obtained, 100~120mL sodium hydroxide solution is added into the xanthate of mulberry skin slag, obtains fiber
Plain viscose;
(5)40~45mL dimethylallylamine is added into the four-hole boiling flask with condensing unit, heat temperature raising is burnt to four mouthfuls
5~7g monoxone and 60~70mL sodium hydroxide solution are added in bottle, are stirred with magnetic stirring apparatus with the revolving speed of 300~400r/min
It being transferred in distilling flask after mixing reaction, heat temperature raising, distillation obtains the suspension containing white crystal, continuously add 100~
110mL dehydrated alcohol is centrifugally separating to obtain the light yellow mucus in upper layer;
(6)The above-mentioned light yellow mucus of 40~50mL and 80~100mL deionization are added into the three-necked flask equipped with condensing unit
Water, then chlorine is passed through into three-necked flask, the pH of reaction system in three-necked flask, heat temperature raising are controlled, distillation continues to three mouthfuls
70~80mL dehydrated alcohol is added in flask, is separated by filtration to obtain thick filtrate;
(7)30~35g cationic hydroxyethyl cellulose is added into thick filtrate, is stirred to react to obtain solid crude product, it will
Solid crude product and cellulose viscose be put into acetic acid methanol solution impregnate 40~50min, be separated by filtration removal filtrate obtain it is wet
Wet glue is put into vacuum oven by glue, dry, is ground up, sieved to obtain salt tolerant higher suspension thickener for coating.
2. a kind of preparation method of salt tolerant higher suspension thickener for coating according to claim 1, it is characterised in that:
Step(1)The Ventilation Rate is 40~50mL/min, and the ventilatory response time is 4~5h, vacuum oven setting temperature
Degree is 70~80 DEG C, and drying time is 6~7h.
3. a kind of preparation method of salt tolerant higher suspension thickener for coating according to claim 1, it is characterised in that:
Step(2)The mass fraction of the sodium hydroxide solution is 15%, and being stirred to react the time is 1~2h, the quality point of hydrochloric acid
Number is 20%, and high speed centrifugation revolving speed is 2000~3000r/min, and the centrifugal treating time is 8~10min, and baking oven set temperature is 60
~70 DEG C, drying time is 4~5h.
4. a kind of preparation method of salt tolerant higher suspension thickener for coating according to claim 1, it is characterised in that:
Step(3)The enzymolysis time is 2~3h, and the mass fraction of sodium hydroxide solution is 30%, and the mass fraction of ammonium hydroxide is
20%, heat temperature raising temperature is 60~65 DEG C, and dropping funel drop rate is 3~5mL/min, and being stirred to react the time is 2~3h.
5. a kind of preparation method of salt tolerant higher suspension thickener for coating according to claim 1, it is characterised in that:
Step(4)The mass fraction of the Adlerika is 25%, and heat temperature raising temperature is 50~55 DEG C, drying time 2
~3h, the mass fraction of sodium hydroxide solution are 20%.
6. a kind of preparation method of salt tolerant higher suspension thickener for coating according to claim 1, it is characterised in that:
Step(5)The heat temperature raising temperature is 55~60 DEG C, and the mass fraction of sodium hydroxide solution is 20%, is stirred to react
Time is 20~30min, and heat temperature raising temperature is 70~80 DEG C, and distillation time is 1.5~2.0h.
7. a kind of preparation method of salt tolerant higher suspension thickener for coating according to claim 1, it is characterised in that:
Step(6)The Ventilation Rate be 30~35mL/min, lead to chlorine control three-necked flask in reaction system pH be 6~
7, heat temperature raising temperature is 80~90 DEG C, and distillation time is 2~3h.
8. a kind of preparation method of salt tolerant higher suspension thickener for coating according to claim 1, it is characterised in that:
Step(7)The time that is stirred to react is 30~40min, and the mass fraction of the methanol solution of acetic acid is 20%, and vacuum is dry
Dry case set temperature is 70~80 DEG C, and drying time is 10~12h, and be sieved specification is 200 mesh.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111875713A (en) * | 2020-07-31 | 2020-11-03 | 董群雄 | Cellulose ether for drilling fluid and preparation method thereof |
| CN116285524A (en) * | 2023-03-20 | 2023-06-23 | 北京东方雨虹防水技术股份有限公司 | Waterproof sound insulation coating and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104970A (en) * | 1986-07-29 | 1988-02-10 | 陈民 | Preparation of Heavy Metal Scavenger from Cellulose-Containing Waste |
| US20080227892A1 (en) * | 2007-03-13 | 2008-09-18 | Van Der Wielen Maarten | Paint formulations comprising cellulose ether/network building polymer fluid gel thickeners |
| CN108164606A (en) * | 2017-12-30 | 2018-06-15 | 江苏华友装饰工程有限公司 | Preparation method of amphoteric cellulose ether for drilling fluid |
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2018
- 2018-07-25 CN CN201810827908.8A patent/CN108864801A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104970A (en) * | 1986-07-29 | 1988-02-10 | 陈民 | Preparation of Heavy Metal Scavenger from Cellulose-Containing Waste |
| US20080227892A1 (en) * | 2007-03-13 | 2008-09-18 | Van Der Wielen Maarten | Paint formulations comprising cellulose ether/network building polymer fluid gel thickeners |
| CN108164606A (en) * | 2017-12-30 | 2018-06-15 | 江苏华友装饰工程有限公司 | Preparation method of amphoteric cellulose ether for drilling fluid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111875713A (en) * | 2020-07-31 | 2020-11-03 | 董群雄 | Cellulose ether for drilling fluid and preparation method thereof |
| CN116285524A (en) * | 2023-03-20 | 2023-06-23 | 北京东方雨虹防水技术股份有限公司 | Waterproof sound insulation coating and application |
| CN116285524B (en) * | 2023-03-20 | 2024-03-12 | 北京东方雨虹防水技术股份有限公司 | Waterproof sound insulation coating and application |
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