CN1049677C - Luke composite fire retarding agent and its production - Google Patents
Luke composite fire retarding agent and its production Download PDFInfo
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- CN1049677C CN1049677C CN95110432A CN95110432A CN1049677C CN 1049677 C CN1049677 C CN 1049677C CN 95110432 A CN95110432 A CN 95110432A CN 95110432 A CN95110432 A CN 95110432A CN 1049677 C CN1049677 C CN 1049677C
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- 239000002131 composite material Substances 0.000 title claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000003340 retarding agent Substances 0.000 title description 5
- 239000002994 raw material Substances 0.000 claims abstract description 19
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 16
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 13
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 8
- 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 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 7
- 239000011734 sodium Substances 0.000 claims abstract description 7
- 241001070941 Castanea Species 0.000 claims abstract description 6
- 235000014036 Castanea Nutrition 0.000 claims abstract description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 241000124033 Salix Species 0.000 claims abstract description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 239000012452 mother liquor Substances 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000012752 auxiliary agent Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- DJOWTWWHMWQATC-KYHIUUMWSA-N Karpoxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1(O)C(C)(C)CC(O)CC1(C)O)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C DJOWTWWHMWQATC-KYHIUUMWSA-N 0.000 claims description 6
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 6
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 6
- QCENGKPIBJNODL-UHFFFAOYSA-N n'-dodecylethane-1,2-diamine Chemical compound CCCCCCCCCCCCNCCN QCENGKPIBJNODL-UHFFFAOYSA-N 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- 102000008186 Collagen Human genes 0.000 claims description 5
- 108010035532 Collagen Proteins 0.000 claims description 5
- 241000218691 Cupressaceae Species 0.000 claims description 5
- 240000005001 Paeonia suffruticosa Species 0.000 claims description 5
- 235000003889 Paeonia suffruticosa Nutrition 0.000 claims description 5
- 229920001436 collagen Polymers 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000001384 succinic acid Substances 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 229940051043 cresylate Drugs 0.000 claims description 3
- 239000012757 flame retardant agent Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 claims description 2
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 3
- 240000006891 Artemisia vulgaris Species 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- 240000001851 Artemisia dracunculus Species 0.000 abstract description 5
- 235000009419 Fagopyrum esculentum Nutrition 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract 3
- 239000010902 straw Substances 0.000 abstract 2
- 235000009051 Ambrosia paniculata var. peruviana Nutrition 0.000 abstract 1
- 235000003097 Artemisia absinthium Nutrition 0.000 abstract 1
- 235000017731 Artemisia dracunculus ssp. dracunculus Nutrition 0.000 abstract 1
- 235000003261 Artemisia vulgaris Nutrition 0.000 abstract 1
- FAHJTGXLUTXMMP-UHFFFAOYSA-N C(CCC(=O)O)(=O)O.C(CCCCCCCCCCC)NCCN Chemical compound C(CCC(=O)O)(=O)O.C(CCCCCCCCCCC)NCCN FAHJTGXLUTXMMP-UHFFFAOYSA-N 0.000 abstract 1
- 235000007871 Chrysanthemum coronarium Nutrition 0.000 abstract 1
- 244000067456 Chrysanthemum coronarium Species 0.000 abstract 1
- 240000008620 Fagopyrum esculentum Species 0.000 abstract 1
- 241000972673 Phellodendron amurense Species 0.000 abstract 1
- 244000062793 Sorghum vulgare Species 0.000 abstract 1
- 241001464837 Viridiplantae Species 0.000 abstract 1
- 239000001138 artemisia absinthium Substances 0.000 abstract 1
- 235000019713 millet Nutrition 0.000 abstract 1
- 238000003541 multi-stage reaction Methods 0.000 abstract 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 abstract 1
- 230000035699 permeability Effects 0.000 abstract 1
- 239000002574 poison Substances 0.000 abstract 1
- 231100000614 poison Toxicity 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 208000011117 substance-related disease Diseases 0.000 abstract 1
- 239000003063 flame retardant Substances 0.000 description 12
- 241000196324 Embryophyta Species 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 244000025254 Cannabis sativa Species 0.000 description 4
- 241000219051 Fagopyrum Species 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- -1 this moment Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Paper (AREA)
Abstract
The present invention belongs to a composite flame-resistance substance with green plants as raw material and a preparation method thereof. The flame-resistance substance uses buckwheat straw, hairy chestnut flower, fragrant crown daisy, millet straw, azedarach, phellodendron bark, cortex moutan, willow root and seleng wormwood as raw material which is extracted by a water solution of phosphoric acid, acetic acid and butanol as an extractant, and then the flame-resistance substance is present by purification and a composite reaction by an NH4 OH water solution, urea, ammonioformaldehyde, pentaerythritol, lauryl alcohol, isopropyl alcohol, tetrachlorotricresol sodium and N-dodecyl ethylenediamine succinic acid. The prepared flame-resistance substance has the advantages of good flame resistance effect, stable performance, low viscosity, strong permeability, no poison and no pollution and simple preparation technology.
Description
The invention belongs to a kind of is the method that raw material is produced the composite flame-proof material with plant.
Existing fire retardant is divided into organic and inorganic two big classes, is pure chemistry method synthetics.The overwhelming majority is non-water-soluble, is restricted in the application.Wherein inorganic combustion inhibitor safe in utilization, be fuming lowly, but flame retardant effect is poor, consumption is big, is unfavorable for the processing of material.Organic fire-retardant is toxic, easily pollutes, and poor stability, and cost height, not ideal enough.
The objective of the invention is to make a kind of flame retarding efficiency height, nontoxic, pollution-free, stable performance, viscosity is low, perviousness is strong, production technique is simple, cost is low water-soluble flame retardant.
The present invention utilizes to contain assorted many lopps organic substance in the natural phant, the splendid composite flame-retardant agent of producing through the complex reaction of extraction, purifying and chemical assistant of flame retardant effect.
The natural phant that the present invention utilized is buckwheat all grass, chestnut flower, fragrant Tong, paddy joint, amargosa bark, golden cypress, the root bark of tree peony, willow root, water wormwood artemisia.Employed extraction agent is the aqueous solution of acetate, phosphoric acid, butanols.Employed auxiliary agent is NH
4Defend tetrol, lauryl alcohol, Virahol, glycerol, tetrachloro three sodium cresylates and N-dodecyl ethylene diamine Succinic Acid in the OH aqueous solution, urea, hexamethylenetetramine, season.
The best proportioning (by weight) of natural plant raw material used in the present invention is: buckwheat all grass 5-15%, chestnut flower 1-5%, fragrant Tong 25-30%, paddy joint 20-40%, amargosa bark 5-8%, golden cypress 5-15%, root bark of tree peony 2-10%, willow root 1.5-3%, water wormwood artemisia 3-8%.For the effective constituent in the plant material is extracted fully, the best proportioning of its raw material and extraction is soaked for the 1Kg raw material needs 16-24 to rise extraction agent.Various components in proportions (by weight) are phosphatase 11 .5-11%, acetate 0.25-5%, butanols 0.25-3%, water 88-98% in its extraction agent, the add-on of other auxiliary agents, for the ease of calculating, all according to the usage quantity of plant material for according to measuring, the ratio that is respectively raw material weight is: urea 50-65%, hexamethylenetetramine 20-30%, defend tetrol 8-15%, lauryl alcohol 1-4%, Virahol 40-60%, glycerol 25-35%, tetrachloro three sodium cresylate 85-100%, N-dodecyl ethylene diamine Succinic Acid 1-4% season.The NH that uses
4The aqueous solution of OH is mainly used to adjust the potential of hydrogen of mother liquor, and its consumption is to decide according to the pH value that the mother liquor after the extracting is adjusted to, and the best pH value of mother liquor was 8-9 after the present invention required to adjust.The same NH of employed phosphoric acid
4The OH aqueous solution is the same, also is to finish the pH value of back mother liquor in order to adjust the first step reaction, and method is that the mother liquor pH value after the filtration is adjusted at 6.1-7.0.
The manufacture method of this plant fire retardant is: at first raw material buckwheat all grass, chestnut flower, golden cypress, the root bark of tree peony, paddy joint, amargosa bark, fragrant Tong, willow root, water wormwood artemisia are pulverized, the degree of its pulverizing is 1-2CM.Raw material after will pulverizing is then put in the extraction agent that is made of phosphoric acid, acetate, the butyro-aqueous solution and is soaked, constantly soaking 24-48 hour under the condition of stirring, filter then, the mother liquor that filters out is placed reactor, constantly slowly adding auxiliary agent NH under the condition of stirring
4The OH aqueous solution makes the potential of hydrogen of mother liquor be transferred to PH8-9, at this moment will produce a large amount of collagen throw outs in the mother liquor, and mother liquor is filtered, and the collagen throw out in the mother liquor is filtered out.Liquid behind the fine filtering is transferred PH6.1-7 with phosphoric acid, puts liquid then again and carry out the reaction of second step in reactor.Liquid heat is arrived 80-90 ℃, under agitation add urea, hexamethylenetetramine, defend tetrol reaction 20-40 minute season, preferably 25-30 minute, add N-dodecyl ethylene diamine Succinic Acid, lauryl alcohol, Virahol, glycerol, tetrachloro three sodium cresylates again, stir to cool off, filter after five minutes and promptly get product.
In the production process of the present invention, the add-on of the proportioning of its proportion of raw materials, raw material and extraction agent, the proportioning of extraction agent itself, various auxiliary agents is preferably according to above-mentioned optimum proportion preparation.About various raw materials, extract dosage, describe in detail more than the amount of auxiliary, just no longer repeat here.Equipment used in the present invention has: stainless steel or enamel reaction still, liquid delivery pump, stationary tank or jar, steam boiler or other heating installations, general pressure filter or plate and frame(type)filter press etc.The selection of its plant material wants quality pure, no rotten.
The present invention's natural phant is a raw material, the fire retardant of producing through extraction, purifying and chemical assistant complex reaction.When acting on combustiblematerials, in liquid phase, gas phase and solid phase, collaborative performance fire retardation, the combustion conditions at destruction interface promotes the solid phase carburizing reagent, reaches fire-retardant purpose, produces fabulous fire-retardant reinforced effects.Through legal detection, this fire retarding agent can reach 48-53 to oxygen index wooden, cotton, and, organic fire-retardant more inorganic than having now exceeds more than 20%.This fire retarding agent can be applicable to the fire-retardant of water-absorbent combustible matl, can adopt soak, method constructions such as spray, brushing.Pollution-free in fire extinguishing, nontoxic.This fire retarding agent can be used for the fire extinguishing of A, category-B fire, especially is suitable for forest extinguishing.The production technique of this fire retardant is simple, safe and reliable, pollution-free, and product viscosity is low, perviousness is strong, stable performance.
Embodiment:
Get in the extraction agent soaking compartment that the buckwheat all grass 2.0Kg, chestnut flower 0.5Kg, fragrant Tong 5.5Kg, paddy joint 6.0Kg, amargosa bark 1.5Kg, golden cypress 2.0Kg, root bark of tree peony 1.0Kg, willow root 0.6Kg, the water wormwood artemisia 1.0Kg that pulverize behind the 1-2cm immerse the aqueous solution that is placed with 400 liters of phosphoric acid, acetate, butanols 2,0-12% and soaked 35 hours, should constantly stir therebetween.Then it is filtered, the red mother liquor that filters out with pump delivery in reactor, slow adding NH under continuous condition of stirring
4The OH aqueous solution, the pH value 8-9 in mother liquor, this moment, solution was deep green, and with a large amount of collagen agent precipitations, the collagen throw out that produces in the mother liquor was filtered out with plate-and-frame filter press.With phosphoric acid liquid is transferred PH6-7 more afterwards.Again put mother liquor in reactor, heat 80-90 ℃, under agitation add urea 12.0Kg, hexamethylenetetramine 5.0Kg, defend tetrol 2.5Kg season, react after 20-30 minute, add N-dodecyl ethylene diamine Succinic Acid 0.5Kg, lauryl alcohol 0.5Kg, Virahol 10.0Kg glycerol 6.0Kg, tetrachloro three sodium cresylate 18.0Kg again, stir five minutes postcooling, filtration, deposit hold tank in.The density of the fire retarding agent product of producing like this is p201.145-1.155, viscosity mp2s (20 ℃) 2.9-3.1, PH6.5-7.5, solid content 〉=15.Its combustionproperty: oxygen index, timber 45-55, cotton 45-53, filter paper 48-56.After flame time 0; Duration of fire resistance S≤5.
Claims (1)
1, the manufacture method of composite flame-retardant agent is characterized in that: with Testa Fagopyri Esculenti 5-15%, chestnut flower 1-5%, fragrant Tong 25-30%, paddy joint 20-40%, amargosa bark 5-8%, golden cypress 5-15%, root bark of tree peony 2-10%, willow root 1.5-3%, water wormwood artemisia 3-8% (by weight) is raw material; Above-mentioned raw materials is crushed to 1-2cm will be mixed with extraction agent by the raw material after pulverizing then, its ratio of mixture rises extraction agent for the 1Kg raw material adds 16-24, and the content of each composition (by weight) is phosphatase 11 .5-11%, acetate 0.25-5%, butanols 0.25-3.0% and water 88-98% in the extraction agent; The mixture of raw material and extraction agent is slowly added NH under condition of stirring
4The OH aqueous solution, make the pH value of mother liquor transfer to 8-9, then the collagen throw out that produces is filtered out, liquid behind the fine filtering transfers pH value to 6.1-7.0 with phosphoric acid, again liquid is placed in the reactor and heat, make the temperature of liquid reach 80-90 ℃, under agitation add auxiliary agent, the add-on of various auxiliary agents all is base value with the weight of used raw material, be respectively the plain 50-65% of urea, hexamethylenetetramine 20-30%, defend tetrol 8-15% season, lauryl alcohol 1-4%, Virahol 40-60%, glycerol 25-35%, tetrachloro three sodium cresylate 85-100%, N-dodecyl ethylene diamine Succinic Acid 1-4%, the order that adds auxiliary agent is: under agitation, add the urea element earlier, hexamethylenetetramine, season is defended tetrol, after making it to react 20-40 minute, add N-dodecyl ethylene diamine Succinic Acid again, lauryl alcohol, different third ferment, glycerol, tetrachloro three sodium cresylates, restir five minutes, cooling, promptly obtain this product after the filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95110432A CN1049677C (en) | 1995-04-28 | 1995-04-28 | Luke composite fire retarding agent and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95110432A CN1049677C (en) | 1995-04-28 | 1995-04-28 | Luke composite fire retarding agent and its production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1118368A CN1118368A (en) | 1996-03-13 |
| CN1049677C true CN1049677C (en) | 2000-02-23 |
Family
ID=5077815
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95110432A Expired - Fee Related CN1049677C (en) | 1995-04-28 | 1995-04-28 | Luke composite fire retarding agent and its production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1049677C (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064487A (en) * | 1991-02-26 | 1992-09-16 | 国际壳牌研究有限公司 | Catalyst composition |
-
1995
- 1995-04-28 CN CN95110432A patent/CN1049677C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064487A (en) * | 1991-02-26 | 1992-09-16 | 国际壳牌研究有限公司 | Catalyst composition |
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| Publication number | Publication date |
|---|---|
| CN1118368A (en) | 1996-03-13 |
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