CN105001911B - A kind of toughness amide waxe and preparation method thereof - Google Patents
A kind of toughness amide waxe and preparation method thereof Download PDFInfo
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- CN105001911B CN105001911B CN201510325171.6A CN201510325171A CN105001911B CN 105001911 B CN105001911 B CN 105001911B CN 201510325171 A CN201510325171 A CN 201510325171A CN 105001911 B CN105001911 B CN 105001911B
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- amide
- alcaminess
- diamine
- acid
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- 150000001408 amides Chemical class 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 21
- 150000004985 diamines Chemical class 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical group O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 34
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 32
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000003963 antioxidant agent Substances 0.000 claims description 16
- 230000003078 antioxidant effect Effects 0.000 claims description 16
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 16
- 150000004668 long chain fatty acids Chemical class 0.000 claims description 13
- -1 alcaminess and in Chemical class 0.000 claims description 9
- 150000002885 octadecanoids Chemical class 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 5
- 235000021314 Palmitic acid Nutrition 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- QVYARBLCAHCSFJ-UHFFFAOYSA-N butane-1,1-diamine Chemical compound CCCC(N)N QVYARBLCAHCSFJ-UHFFFAOYSA-N 0.000 claims description 2
- PWSKHLMYTZNYKO-UHFFFAOYSA-N heptane-1,7-diamine Chemical compound NCCCCCCCN PWSKHLMYTZNYKO-UHFFFAOYSA-N 0.000 claims description 2
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 2
- KJOMYNHMBRNCNY-UHFFFAOYSA-N pentane-1,1-diamine Chemical compound CCCCC(N)N KJOMYNHMBRNCNY-UHFFFAOYSA-N 0.000 claims description 2
- GGHDAUPFEBTORZ-UHFFFAOYSA-N propane-1,1-diamine Chemical compound CCC(N)N GGHDAUPFEBTORZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 125000002252 acyl group Chemical group 0.000 claims 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000002530 phenolic antioxidant Substances 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 230000004992 fission Effects 0.000 abstract description 7
- 239000000155 melt Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 229940043237 diethanolamine Drugs 0.000 description 28
- 239000001993 wax Substances 0.000 description 19
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 235000021355 Stearic acid Nutrition 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 3
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 235000019260 propionic acid Nutrition 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910052756 noble gas Inorganic materials 0.000 description 2
- 150000002835 noble gases Chemical class 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- FEXBEKLLSUWSIM-UHFFFAOYSA-N 2-Butyl-4-methylphenol Chemical compound CCCCC1=CC(C)=CC=C1O FEXBEKLLSUWSIM-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- KYYWBEYKBLQSFW-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCC(O)=O KYYWBEYKBLQSFW-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 150000004667 medium chain fatty acids Chemical class 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- ZTUXEFFFLOVXQE-UHFFFAOYSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCC(O)=O ZTUXEFFFLOVXQE-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- Lubricants (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of toughness amide waxe and preparation method thereof, belong to synthetic wax technical field.The present invention with amide-type and/or diamine, alcaminess and in, long-chain fat acid substance is as raw material, under base catalyst effect, 130～170 DEG C are reacted 1～5 hour, the melt drop temperature of synthesis toughness amide waxe is between 60～90 DEG C, under room temperature, film (thickness 1mm) bends 0～120 degree and does not fission, good properties.In the present invention, the preparation method of toughness amide waxe is simple, easy to operate, and raw material sources are extensive and cheap, and the property of toughness wax can be adjusted flexibly according to the actual requirements.
Description
Technical field
The present invention relates to a kind of toughness amide waxe, also relate to the preparation method of this toughness amide waxe, belong to synthetic wax
Technical field.
Background technology
Pertroleum wax is a kind of solid hydrocarbon mixture obtaining from petroleum refining, can be widely used for plastics, rubber, papermaking,
Ink, daily-use chemical industry, weaving, the field such as agriculture and mechanical.With the development of social progress and industrial technology, wax is in other industry
And the demand in emerging field is also continuously increased, such as national defense industry, high-grade wax candle, poultry epilation, dentistry and slow release fertilizer etc., right
The performance of wax product has higher requirement (as toughness, hardness etc.) so that original paraffin wax product can not meet modern work
The demand of industry.
The toughness of wax refers to the pliability after wax film forming, and toughness is better, occurs the probability of brittle fracture less.Abroad
Mainly oil toughness wax is prepared by residual oil slack wax removing oil.Residual oil slack wax obtains No. 85 microwaxes through three sections of removing oils, and its filtrate is again
Removing oil obtains No. 65 toughness waxes, and No. 65 wax filtrates refilter and obtain No. 55 toughness waxes.Various products can be pressed difference by above-mentioned technique
Ratio is in harmonious proportion and obtains the microwax of 75～85 DEG C of dropping point and the toughness wax of 55～70 DEG C of dropping point.
Amide waxe is one of staple product in synthetic wax, is obtained by fatty-acylation, such as the carboxylic acid of 12 carbon or 18 carbon
React with primary amine, secondary amine, tertiary amine, quaternary amine and ethanolamine.The feature of amide waxe is that fusing point is high, up to more than 90 DEG C, but
Toughness is poor.Domestic and foreign literature is related to Toughness Improvements of Polyamide and the report of toughness alkanolamide, it is known from literature that polyamide
Elastomer good toughness, but its complex process, operating difficultiess, and polyamide molecular weight is big, fusing point is high.Although toughness alkanolamide wax
Molecular weight is little, but fusing point is relatively low, generally below 60 DEG C.
Content of the invention
It is an object of the invention to provide a kind of toughness amide waxe.
Meanwhile, the present invention also provides a kind of preparation method of toughness amide waxe.
In order to realize object above, the technical solution adopted in the present invention is：
A kind of toughness amide waxe, with amide-type and/or diamine, alcaminess and in, long-chain fatty acid closes for raw material reaction
Become.
In terms of mass fraction, each raw material dosage is：18～46 parts of amide-type and/or 1～12 part of diamine, alcaminess 2～
26 parts, in, 30～70 parts of long-chain fatty acid.
Described amide-type is caprolactam；Described diamine be dimethyl-penten diamidogen, ethylenediamine, propane diamine, butanediamine,
Any one or more in pentanediamine, hexamethylene diamine, heptamethylene diamine, dodecane diamine, p-phenylenediamine.Described diamine is mainly
Refer to the amino-compound containing two amino.
Described alcaminess are one or more of monoethanolamine, diethanolamine, triethanolamine.Be preferably monoethanolamine and
Diethanolamine.
In described, (it is 6～12 that medium-chain fatty acid refers to carbon number in carbochain to long-chain fatty acid, and long-chain fatty acid refers to carbochain
Upper carbon number be more than 12) include dodecylic acid (lauric acid), tetradecanoic acid (myristic acid), hexadecanoic acid (palmitic acid), ten
Eight alkanoic acids (stearic acid) etc..It is preferably octadecanoid acid.
Preferably, described amide-type is caprolactam, and described alcaminess are monoethanolamine and diethanolamine, described in, long
Chain fatty acid is octadecanoid acid.
In terms of mass fraction, each raw material dosage is：18～46 parts of caprolactam, 1～13 part of monoethanolamine, diethanolamine 1
～13 parts, 30～70 parts of octadecanoid acid.
The catalyst that described synthesis (reaction) adopts is base catalyst, such as potassium hydroxide, sodium hydroxide, Lithium hydrate etc.
In any one.In terms of mass fraction, the consumption of catalyst is 0.1～3 part.
In described synthetic reaction, antioxidant is Hinered phenols antioxidant.Described Hinered phenols antioxidant is 2,6- three-level fourth
Base -4- methylphenol, double (3,5- three-level butyl -4- hydroxy phenyl) thioether, four (β-(3,5- three-level butyl -4- hydroxy phenyls)
Propanoic acid) in any one.In terms of mass fraction, the consumption of antioxidant is 0～1.5 part.Above-mentioned antioxidant can lead to generation in Yantai
Work company limited buys.
The temperature of described synthesis (reaction) is 130～170 DEG C, and the response time is 1～5 hour.
A kind of preparation method of above-mentioned toughness amide waxe it is characterised in that：Comprise the following steps：
(1) by amide-type and/or diamine, alcaminess, in, long-chain fatty acid mix with antioxidant, in noble gases atmosphere
It is warming up to 130～170 DEG C in enclosing, react 1～2 hour；
In terms of mass fraction, each raw material dosage is：18～46 parts of amide-type and/or 1～12 part of diamine, alcaminess 2～
26 parts, 0～1.5 part of antioxidant；
(2) reaction finishes, and is cooled to 135～160 DEG C, adds alcaminess, adds catalyst, in 135～165 DEG C of temperature
Under react to product acid number be 1～12KOHmg/g, obtain final product；
In terms of mass fraction, each raw material dosage is：0～10 part of alcaminess, 0.1～3 part of catalyst.
Preferably, a kind of preparation method of toughness amide waxe, comprises the following steps：
(1) caprolactam, monoethanolamine, diethanolamine, octadecanoid acid are mixed with antioxidant, in atmosphere of inert gases
It is warming up to 130～170 DEG C, react 1～2 hour；
In terms of mass fraction, each raw material dosage is：18～46 parts of caprolactam, 1～8 part of monoethanolamine, diethanolamine 1～
8 parts, 0～1.5 part of antioxidant；
(2) reaction finishes, and is cooled to 135～165 DEG C, adds monoethanolamine and/or diethanolamine, adds catalyst,
Reacting at 135～165 DEG C of temperature to product acid number is 1～12KOHmg/g, obtains final product；
In terms of mass fraction, each raw material dosage is：0～5 part of monoethanolamine, 0～5 part of diethanolamine, catalyst 0.1～3
Part, it is 0 when monoethanolamine is different from the consumption of diethanolamine.
In described step (1), noble gases are nitrogen.
Beneficial effects of the present invention：
The present invention with amide-type, alcaminess and in, long-chain fatty acid as raw material, the melt drop temperature of synthesis toughness amide waxe is 60
Between～90 DEG C, under room temperature, film (thickness 1mm) bends 0～120 degree and does not fission, good properties.
In the present invention, the preparation method of toughness amide waxe is simple, easy to operate, and raw material sources are extensive and cheap, can basis
Actual demand is adjusted flexibly the property of toughness wax.
Specific embodiment
Following embodiments are only described in further detail to the present invention, but do not constitute any limitation of the invention.
Embodiment 1
In the present embodiment, toughness amide waxe is former with ethylenediamine, caprolactam, monoethanolamine, diethanolamine and dodecylic acid
Material is synthesized；In mass, each raw material dosage is：3 grams of ethylenediamine, caprolactam 23.3g, monoethanolamine 3.1g, diethanol
Amine 2g, dodecylic acid 65.5g.
In the present embodiment, the preparation method of toughness amide waxe, comprises the following steps：
(1) by 3 grams of ethylenediamine, monoethanolamine 1.1g, diethanolamine 1g, dodecylic acid 65.5g and antioxidant 2,6- three-level
Butyl -4- methylphenol 0.5g adds in the four-hole boiling flask with agitator, thermocouple and condensing tube, is passed through nitrogen, is warming up to
170 DEG C, react 1 hour；
(2) reaction finishes, and is cooled to 135 DEG C, adds monoethanolamine 2g, diethanolamine 1g and potassium hydroxide 0.7g, in temperature
React 4 hours at 135 DEG C of degree, obtain toughness amide waxe.
Toughness amide waxe manufactured in the present embodiment is white solid, and melt drop temperature is 76 DEG C, and acid number is 4.5KOHmg/g, amine number
For 34.5KOHmg/g, film (thickness 1mm) bends 90 degree and does not fission at normal temperatures.
Embodiment 2
In the present embodiment, toughness amide waxe is closed with hexamethylene diamine, monoethanolamine, diethanolamine and tetradecanoic acid for raw material reaction
Become；In mass, each raw material dosage is：1 gram of hexamethylene diamine, monoethanolamine 13g, diethanolamine 11g, tetradecanoic acid 30g.
In the present embodiment, the preparation method of toughness amide waxe, comprises the following steps：
(1) by 1 gram of hexamethylene diamine, double (3, the 5- three-level fourths of monoethanolamine 8g, diethanolamine 6g, tetradecanoic acid 30g and antioxidant
Base -4- hydroxy phenyl) thioether 0.6g add with agitator, thermocouple and condensing tube four-hole boiling flask in, be passed through nitrogen, heat up
To 150 DEG C, react 2 hours；
(2) reaction finishes, and is cooled to 150 DEG C, adds monoethanolamine 5g, diethanolamine 5g and potassium hydroxide 0.1g, in temperature
React 3 hours at 150 DEG C of degree, obtain toughness amide waxe.
Toughness amide waxe manufactured in the present embodiment is white solid, and melt drop temperature is 80 DEG C, and acid number is 4.5KOHmg/g, amine number
For 40.5KOHmg/g, film (thickness 1mm) bends 90 degree and does not fission at normal temperatures.
Embodiment 3
In the present embodiment, toughness amide waxe is former with certain herbaceous plants with big flowers diamidogen, caprolactam, monoethanolamine, diethanolamine and hexadecanoic acid
Material is synthesized；In mass, each raw material dosage is：12 grams of certain herbaceous plants with big flowers diamidogen, caprolactam 25g, monoethanolamine 9g, diethanolamine
8g, hexadecanoic acid 36.9g.
In the present embodiment, the preparation method of toughness amide waxe, comprises the following steps：
(1) 12 grams of certain herbaceous plants with big flowers diamidogen, caprolactam 25g, monoethanolamine 8g, diethanolamine 4g and hexadecanoic acid 36.9g are added
In four-hole boiling flask with agitator, thermocouple and condensing tube, it is passed through nitrogen, is warming up to 130 DEG C, react 2 hours；
(2) reaction finishes, and is cooled to 135 DEG C, adds monoethanolamine 5g and potassium hydroxide 0.1g, anti-at 135 DEG C of temperature
Answer 4 hours, obtain toughness amide waxe.
Toughness amide waxe manufactured in the present embodiment is white solid, and melt drop temperature is 87 DEG C, and acid number is 4.5KOHmg/g, amine number
For 47.6KOHmg/g, film (thickness 1mm) bends 90 degree and does not fission at normal temperatures.
Embodiment 4
In the present embodiment, toughness amide waxe is former with hexamethylene diamine, caprolactam, monoethanolamine, diethanolamine and octadecanoid acid
Material is synthesized；In mass, each raw material dosage is：5 grams of hexamethylene diamine, caprolactam 13.5g, monoethanolamine 4g, diethanolamine
13g, octadecanoid acid 60g.
In the present embodiment, the preparation method of toughness amide waxe, comprises the following steps：
(1) by 5 grams of hexamethylene diamine, caprolactam 13.5g, monoethanolamine 4g, diethanolamine 8g, octadecanoid acid 60g and antioxygen
Agent four (β-(3,5- three-level butyl -4- hydroxy phenyl) propanoic acid) 1.5g adds four mouthfuls with agitator, thermocouple and condensing tube
In flask, it is passed through nitrogen, is warming up to 160 DEG C, react 2 hours；
(2) reaction finishes, and is cooled to 165 DEG C, adds diethanolamine 5g and potassium hydroxide 3g, reacts 3 at 165 DEG C of temperature
Hour, obtain toughness amide waxe.
Toughness amide waxe manufactured in the present embodiment is white solid, and melt drop temperature is 86 DEG C, and acid number is 4.8KOHmg/g, amine number
For 33.2KOHmg/g, film (thickness 1mm) bends 90 degree and does not fission at normal temperatures.
Embodiment 5
In the present embodiment, toughness amide waxe is former with p-phenylenediamine, caprolactam, monoethanolamine, diethanolamine and stearic acid
Material is synthesized；In mass, each raw material dosage is：8 grams of p-phenylenediamine, caprolactam 20g, monoethanolamine 2.7g, diethanol
Amine 7g, stearic acid 70g.
In the present embodiment, the preparation method of toughness amide waxe, comprises the following steps：
(1) by 8 grams of p-phenylenediamine, caprolactam 10g, monoethanolamine 2.2g, diethanolamine 6g, stearic acid 70g and antioxygen
Agent four (β-(3,5- three-level butyl -4- hydroxy phenyl) propanoic acid) 0.1g adds four mouthfuls with agitator, thermocouple and condensing tube
In flask, it is passed through nitrogen, is warming up to 170 DEG C, react 1 hour；
(2) reaction finishes, and is cooled to 145 DEG C, adds monoethanolamine 1g, diethanolamine 0.5g and potassium hydroxide 0.2g,
React 4 hours at 145 DEG C of temperature, obtain toughness amide waxe.
Toughness amide waxe manufactured in the present embodiment is white solid, and melt drop temperature is 85 DEG C, and acid number is 3.2KOHmg/g, amine number
For 32.6KOHmg/g, film (thickness 1mm) bends 90 degree and does not fission at normal temperatures.
10 grams of Example 5 gained toughness amide wax product, 30 grams of No. 58 paraffin wax fully refineds, in 120 degree of whipping temp
Under, mix and blend 30 minutes, it is subsequently poured in molding device.After mixture cools down, observe and find the two mix homogeneously, do not send out
Existing lamination, shows prepared toughness wax and paraffin good mixing.
Claims (9)
1. a kind of toughness amide waxe it is characterised in that：With amide-type and/or diamine, alcaminess and in, long-chain fatty acid
For raw material reaction synthesis；In terms of mass fraction, each raw material dosage is：18 ~ 46 parts of amide-type and/or diamine 1 ~
12 parts, 2 ~ 26 parts of alcaminess, in, 30 ~ 70 parts of long-chain fatty acid；Described toughness amide waxe is to be prepared by following methods
's：
（1）By amide-type and/or diamine, alcaminess, in, long-chain fatty acid mix with antioxidant, in atmosphere of inert gases
It is warming up to 130～170 DEG C, react 1～2 hour；
In terms of mass fraction, each raw material dosage is：18～46 parts of amide-type and/or 1～12 part of diamine, alcaminess 2～26
Part, 0～1.5 part of antioxidant；
（2）Reaction finishes, and is cooled to 135～160 DEG C, adds alcaminess, adds catalyst, anti-at 135～165 DEG C of temperature
Should be 1～12 KOHmg/g to product acid number, obtain final product；
In terms of mass fraction, each raw material dosage is：0～10 part of alcaminess, 0.1～3 part of catalyst.
2. the toughness amide waxe according to claim 1 it is characterised in that：Described amide-type is caprolactam；Institute
Stating diamine is dimethyl-penten diamidogen, ethylenediamine, propane diamine, butanediamine, pentanediamine, hexamethylene diamine, heptamethylene diamine, dodecane
Any one or more in diamine, p-phenylenediamine.
3. the toughness amide waxe according to claim 1 it is characterised in that：Described alcaminess are monoethanolamine, diethyl
One or more of hydramine, triethanolamine.
4. the toughness amide waxe according to claim 1 it is characterised in that：In described, long-chain fatty acid be dodecane
One or more of acid, tetradecanoic acid, hexadecanoic acid, octadecanoid acid.
5. the toughness amide waxe according to any one of Claims 1 to 4 it is characterised in that：Described amide-type is acyl in oneself
Amine, described alcaminess be monoethanolamine and diethanolamine, described in, long-chain fatty acid be octadecanoid acid.
6. the toughness amide waxe according to claim 1 it is characterised in that：In described synthetic reaction, catalyst is hydrogen-oxygen
Change potassium, sodium hydroxide, in Lithium hydrate any one.
7. the toughness amide waxe according to claim 1 it is characterised in that：In described synthetic reaction, antioxidant is to be obstructed
Phenolic antioxidant.
8. the toughness amide waxe according to claim 1 it is characterised in that：The temperature of described synthetic reaction is 130～170
DEG C, the response time is 1～5 hour.
9. a kind of preparation method of the toughness amide waxe as described in claim 1 it is characterised in that：Comprise the following steps：
（1）By amide-type and/or diamine, alcaminess, in, long-chain fatty acid mix with antioxidant, in atmosphere of inert gases
It is warming up to 130～170 DEG C, react 1～2 hour；
In terms of mass fraction, each raw material dosage is：18～46 parts of amide-type and/or 1～12 part of diamine, alcaminess 2～26
Part, 0～1.5 part of antioxidant；
（2）Reaction finishes, and is cooled to 135～160 DEG C, adds alcaminess, adds catalyst, anti-at 135～165 DEG C of temperature
Should be 1～12 KOHmg/g to product acid number, obtain final product；
In terms of mass fraction, each raw material dosage is：0～10 part of alcaminess, 0.1～3 part of catalyst.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3538032A (en) * | 1967-06-21 | 1970-11-03 | Chevron Res | Wax-amine containing terpolymer compositions for aluminum coating |
| CN1088100C (en) * | 1999-09-29 | 2002-07-24 | 中国石油化工集团公司 | Water-series wax-base lubricant and its preparing process |
| DE10224847B4 (en) * | 2002-06-05 | 2006-04-13 | Clariant Gmbh | Reaction products of mixtures of long-chain fatty acids and aliphatic diamines and their use |
| JP2006188467A (en) * | 2005-01-07 | 2006-07-20 | Nof Corp | Amide wax, method for producing the same, and toner containing the amide wax |
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