CN103352367B - Cold water instant weak cation soft sheet and preparation method thereof - Google Patents
Cold water instant weak cation soft sheet and preparation method thereof Download PDFInfo
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- CN103352367B CN103352367B CN201310211862.4A CN201310211862A CN103352367B CN 103352367 B CN103352367 B CN 103352367B CN 201310211862 A CN201310211862 A CN 201310211862A CN 103352367 B CN103352367 B CN 103352367B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 193
- 150000001768 cations Chemical class 0.000 title claims abstract description 133
- 238000002360 preparation method Methods 0.000 title claims abstract description 60
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 194
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 194
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 194
- 239000008117 stearic acid Substances 0.000 claims abstract description 194
- 238000006243 chemical reaction Methods 0.000 claims abstract description 164
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 144
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 121
- 239000002253 acid Substances 0.000 claims abstract description 113
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000002994 raw material Substances 0.000 claims abstract description 48
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 155
- 238000003756 stirring Methods 0.000 claims description 131
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 126
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 claims description 119
- 229960000583 acetic acid Drugs 0.000 claims description 77
- 239000012362 glacial acetic acid Substances 0.000 claims description 76
- 229910052757 nitrogen Inorganic materials 0.000 claims description 63
- 239000007788 liquid Substances 0.000 claims description 46
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 23
- 238000004458 analytical method Methods 0.000 claims description 22
- 238000009413 insulation Methods 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000004383 yellowing Methods 0.000 abstract description 26
- 238000004519 manufacturing process Methods 0.000 abstract description 24
- 238000000034 method Methods 0.000 abstract description 19
- 239000011259 mixed solution Substances 0.000 abstract 4
- MXBCYQUALCBQIJ-RYVPXURESA-N (8s,9s,10r,13s,14s,17r)-13-ethyl-17-ethynyl-11-methylidene-1,2,3,6,7,8,9,10,12,14,15,16-dodecahydrocyclopenta[a]phenanthren-17-ol;(8r,9s,13s,14s,17r)-17-ethynyl-13-methyl-7,8,9,11,12,14,15,16-octahydro-6h-cyclopenta[a]phenanthrene-3,17-diol Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1.C1CC[C@@H]2[C@H]3C(=C)C[C@](CC)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 MXBCYQUALCBQIJ-RYVPXURESA-N 0.000 abstract 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 abstract 2
- 239000002518 antifoaming agent Substances 0.000 abstract 2
- JVKAWJASTRPFQY-UHFFFAOYSA-N n-(2-aminoethyl)hydroxylamine Chemical compound NCCNO JVKAWJASTRPFQY-UHFFFAOYSA-N 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000004744 fabric Substances 0.000 description 29
- 229920000742 Cotton Polymers 0.000 description 25
- 238000009434 installation Methods 0.000 description 22
- 239000000243 solution Substances 0.000 description 15
- 238000004043 dyeing Methods 0.000 description 3
- -1 cation fatty acid Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000002152 alkylating effect Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000002752 cationic softener Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 229940043237 diethanolamine Drugs 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000346 nonvolatile oil Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a cold water instant weak cation soft sheet and a preparation method thereof. There is no weak cation soft sheet which can be rapidly dissolved in cold water and has low yellowing. The raw materials of the cold water instant weak cation soft sheet comprise, by weight, 68-72 parts of stearic acid, 0.5-1.0 part of phosphorous acid, 7.0-9.0 parts of diethylenetriamine, 8-10 parts of hydroxyethylenediamine, 5.5-6.5 parts of an emulsifier, 6-6.5 parts of acetate acid gracial and 0.5-0.6 parts of an antifoaming agent. The preparation method comprises the following steps: weighing the raw materials; heating a reaction bottle to 80-85DEG C, adding stearic acid to the reaction bottle, and adding phosphorous acid to the reaction bottle to obtain a mixed solution A; adding diethylenetriamine and hydroxyethylenediamine to the mixed solution A to obtain a mixed solution B; and adding the emulsifier, acetate acid gracial and the antifoaming agent to the mixed solution B to obtain the soft sheet. The method has the advantages of simplicity, easy operation and low production cost.
Description
Technical field
The present invention relates to a kind of weak cation flexible sheet and preparation method thereof, especially relate to a kind of cold water instant weak cation soft sheet and preparation method thereof, mainly as the softener of textile printing and dyeing processing, soft finish can be carried out to fiber, fabric.
Background technology
Pure cotton fiber yarn or fabric generally all need through pre-treatment of scouringing and bleaching, and remove the commensals such as wax contained by natural fabric and grease, cause fabric to produce more coarse feel.In order to make fabric have lasting, soft feel, generally all require to carry out soft treatment after dyeing.Use surfactant mainly cationic softener more widely, cheap CATION flexible sheet occupies very large ratio in softener, printing and dyeing mill changes into emulsion film and uses, but these flexible sheets all could will dissolve in the hot water of 70-80 DEG C, the material time is long, waste energy, and xanthochromia degree is high, flatness is poor.
Also some performances relatively better soft of CATION is had at present, if publication date is on 06 09th, 2010, publication number is in the Chinese patent of CN101725043A, disclose a kind of low-temperature instant flexible sheets and preparation method thereof, this low-temperature instant flexible sheets is made up of the raw material of following parts by weight: stearic acid 60-65 part, hydroxyethylethylene diamine 10-15 part, diethylenetriamine 9-16 part, urea 3-5 part, dimethyl carbonate 4-8 part, although this low-temperature instant flexible sheets is can at dissolution in low temperature, low-yellowing, but flatness is slightly poor, it is dark that manufacture process conditional controls the color of bad.And for example publication date on December 14th, 2011, publication number is in the Chinese patent of CN102277739A, disclose a kind of preparation method of weak cation fatty acid softening agent, this preparation method comprises the following steps: fixed oil is heated to fusing, after adding antioxidant, diethylenetriamine is added above-mentioned fused solution, then add hydroxyethylethylene diamine, diethanol amine successively, after intensification, carry out amidatioon condensation reaction and ester exchange reaction; In the product of described amide condensed reaction, add alkylating reagent acetic acid and formic acid, carry out alkylation reaction, then cool blowing section, although make, this softener xanthochromia of sheet softener is low, good hand touch, but solution temperature is high, the material time is long, loses time and the energy.
Also do not have one can dissolve rapidly in cold water now, low-yellowing, soft smooth, biological degradability is good, is applicable to cold water instant weak cation soft sheet of cotton fiber and BLENDED FABRIC soft finish thereof and preparation method thereof.
Summary of the invention
The object of the invention is to overcome above shortcomings in prior art, and provide one to dissolve rapidly in cold water, low-yellowing is soft smooth, biological degradability is good, is applicable to cold water instant weak cation soft sheet of cotton fiber and BLENDED FABRIC soft finish thereof and preparation method thereof.
The present invention's adopted technical scheme that solves the problem is: the feature of this cold water instant weak cation soft sheet is: the raw material of this cold water instant weak cation soft sheet comprises the stearic acid that parts by weight are 68-72 part, parts by weight are the phosphorous acid of 0.5-1.0 part, parts by weight are the diethylenetriamine of 7.0-9.0 part, parts by weight are the hydroxyethylethylene diamine of 8-10 part, parts by weight are the emulsifying agent of 5.5-6.5 part, the defrother of parts by weight to be the glacial acetic acid of 6-6.5 part and parts by weight be 0.5-0.6 part.Make the cold water instant weak cation soft sheet in the present invention can dissolve rapidly in cold water thus, there is low-yellowing, soft smooth, feature that biological degradability is good, be applicable to the soft finish of cotton fiber and BLENDED FABRIC thereof.Cold water instant weak cation soft sheet joins in cold water, under agitation can dissolve rapidly, and mass percentage is the pH value of the aqueous solution of 5% is 4.5-6.
As preferably, stearic acid of the present invention is stearic acid 1801 or stearic acid 1840.
As preferably, emulsifying agent of the present invention is peregal O-25 or emulsifying agent IW.
As preferably, the purity of diethylenetriamine of the present invention and hydroxyethylethylene diamine is all at mass percentage more than 99.0%.
In the present invention, the feature of the preparation method of cold water instant weak cation soft sheet is: described preparation method in turn includes the following steps:
(1) take stearic acid that parts by weight are 68-72 part, glacial acetic acid that emulsifying agent that hydroxyethylethylene diamine that diethylenetriamine that phosphorous acid that parts by weight are 0.5-1.0 part, parts by weight are 7.0-9.0 part, parts by weight are 8-10 part, parts by weight are 5.5-6.5 part, parts by weight are 6-6.5 part and parts by weight are that the defrother of 0.5-0.6 part is as raw material;
(2) reaction bulb is heated to 80-85 DEG C, under the condition stirred, the stearic acid in step (1) is added in reaction bulb, keep the temperature of 80-85 DEG C, stir 20-30 minute, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stir 3-5 minute, phosphorous acid and stearic acid are mixed, thus obtained mixed liquor A;
(3) under the condition opening nitrogen protection, first successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted, after diethylenetriamine and hydroxyethylethylene diamine add, be warmed up to 145-150 DEG C, insulation 0.5-1 hour, at this moment the water-band that reaction generates goes out by nitrogen, is then heated to 200-210 DEG C, reaction 2-3 hour; Sample analysis surveys acid number again, when acid number is less than or equal to 5, meets the requirements, reacts complete, when acid number is greater than 5, continues reaction until acid number meets the requirements; After acid number meets the requirements, cool to 105-110 DEG C, thus obtained mixed liquid B;
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 90-95 DEG C, stir 15-20 minute, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, obtained cold water instant weak cation soft sheet.
Make the preparation method of the cold water instant weak cation soft sheet in the present invention simple thus, processing ease, does not need special installation, and reaction condition is gentle, and production cost is low.
As preferably, stearic acid of the present invention is stearic acid 1801 or stearic acid 1840.
As preferably, emulsifying agent of the present invention is peregal O-25 or emulsifying agent IW.
As preferably, the purity of diethylenetriamine of the present invention and hydroxyethylethylene diamine is all at mass percentage more than 99.0%.
The present invention compared with prior art, has the following advantages and effect: cold water instant weak cation soft sheet can be dissolved rapidly in cold water, has low-yellowing, soft smooth, and biological degradability is good, is applicable to cotton fiber and BLENDED FABRIC soft finish thereof.
In the present invention, the preparation method of cold water instant weak cation soft sheet is simple, and processing ease, does not need special installation, and reaction condition is gentle, and production cost is low.
Detailed description of the invention
Below by embodiment, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 70.5 parts is 0.5 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7 parts, parts by weight are 9 parts, parts by weight are 6 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.5 part, wherein, stearic acid is stearic acid 1801, emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The defrother of the emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that in the present invention, the raw material of cold water instant weak cation soft sheet can comprise stearic acid that parts by weight are 68-72 part, parts by weight are 0.5-1.0 part, parts by weight are 7.0-9.0 part, parts by weight are 8-10 part, parts by weight are 5.5-6.5 part, parts by weight to be the glacial acetic acid of 6-6.5 part and parts by weight be 0.5-0.6 part.Wherein, stearic acid can be the one in stearic acid 1801 and stearic acid 1840, and emulsifying agent can be the one in peregal O-25 and emulsifying agent IW.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 70.5 parts is 0.5 part, parts by weight are 7 parts, parts by weight are 9 parts, parts by weight are 6 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.5 part is as raw material, wherein, stearic acid is stearic acid 1801, emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 80 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 80 DEG C to stir 20 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 3 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; stir in course of reaction; and open a little nitrogen and protect; be warmed up to 145 DEG C of insulations 0.6 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 200 DEG C of reactions 2 hours are heated to, still by nitrogen protection in this course of reaction.Sample analysis surveys acid number, when acid number is less than or equal to 5, reacts complete, meets the requirements; When acid number is greater than 5, continue reaction, until acid number meets the requirements; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.Because stearic acid and amine exothermic heat of reaction, so diethylenetriamine and hydroxyethylethylene diamine need being added in the mixed liquor A of step (2) slowly.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 90 DEG C to stir 15 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.Under stirring in the present invention, section refers in slicing processes to stir and makes composition before and after sheet softener consistent, and this belongs to common practise.
The cold water instant weak cation soft sheet that the present embodiment step (4) obtains joins in cold water, just can dissolve rapidly under stirring, and after dissolving, mass percentage is the aqueous solution of 5%, and its pH value is at 5-6.Cold water instant weak cation soft sheet in the present invention joins in cold water can dissolve rapidly, and such as 50g flexible sheet is placed in the water that 950ml temperature is 30 DEG C, and craft glass bar stirs a minutes and just can dissolve completely.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 2.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 71 parts is 0.5 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.1 parts, parts by weight are 8.4 parts, parts by weight are 6 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.5 part.Wherein, stearic acid is stearic acid 1801, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 71 parts is 0.5 part, parts by weight are 7.1 parts, parts by weight are 8.4 parts, parts by weight are 6 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.5 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 81 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 81 DEG C to stir 21 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 3 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 146 DEG C of insulations 0.7 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 200 DEG C of reactions 2 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 108 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, temperature 92 DEG C is kept to stir 16 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that the present embodiment step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 3.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 71 parts is 0.6 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.2 parts, parts by weight are 8.7 parts, parts by weight are 6 parts, parts by weight to be the glacial acetic acid of 6.4 parts and parts by weight the be defrother of 0.5 part, wherein, stearic acid is stearic acid 1801, emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 71 parts is 0.6 part, parts by weight are 7.2 parts, parts by weight are 8.7 parts, parts by weight are 6 parts, parts by weight are the glacial acetic acid of 6.4 parts and parts by weight is that the defrother of 0.5 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 82 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 82 DEG C to stir 22 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 147 DEG C of insulations 0.7 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 201 DEG C of reactions 2.1 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 93 DEG C to stir 16 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 4.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 71.4 parts is 0.6 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 8 parts, parts by weight are 8 parts, parts by weight are 5.5 parts, parts by weight to be the glacial acetic acid of 6 parts and parts by weight the be defrother of 0.5 part, wherein, stearic acid is stearic acid 1801, emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 71.4 parts is 0.6 part, parts by weight are 8 parts, parts by weight are 8 parts, parts by weight are 5.5 parts, parts by weight are the glacial acetic acid of 6 parts and parts by weight is that the defrother of 0.5 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 83 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 83 DEG C to stir 22 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 148 DEG C of insulations 0.8 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 202 DEG C of reactions 2.5 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, then cool to 109 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 99 DEG C to stir 18 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 5.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 70.5 parts is 0.5 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7 parts, parts by weight are 9 parts, parts by weight are 6 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.5 part, wherein, stearic acid is stearic acid 1840, emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 70.5 parts is 0.5 part, parts by weight are 7 parts, parts by weight are 9 parts, parts by weight are 6 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.5 part is as raw material.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 85 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 85 DEG C to stir 20 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 3 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 145 DEG C of insulations 0.6 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 205 DEG C of reactions 2.3 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 109 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 90 DEG C to stir 15 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 6.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 70.5 parts is 0.5 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7 parts, parts by weight are 9 parts, parts by weight are 6 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.5 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 70.5 parts is 0.5 part, parts by weight are 7 parts, parts by weight are 9 parts, parts by weight are 6 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.5 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 84 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 84 DEG C to stir 25 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 5 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 148 DEG C of insulations 0.8 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 204 DEG C of reactions 2.6 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, then cool to 107 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 93 DEG C to stir 18 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 7.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 69.5 parts is 0.6 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.5 parts, parts by weight are 9.5 parts, parts by weight are 6.4 parts, parts by weight to be the glacial acetic acid of 6 parts and parts by weight the be defrother of 0.5 part.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 69.5 parts is 0.6 part, parts by weight are 7.5 parts, parts by weight are 9.5 parts, parts by weight are 6.4 parts, parts by weight are the glacial acetic acid of 6 parts and parts by weight is that the defrother of 0.5 part is as raw material.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 85 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 85 DEG C to stir 21 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 146 DEG C of insulations 0.9 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 207 DEG C of reactions 2.4 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, when acid number is less than or equal to 5, meets the requirements, reacts complete, when acid number is greater than 5, continues reaction, until acid number meets the requirements; After meeting the requirements Deng acid number, cool to 105 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 95 DEG C to stir 17 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 8.
The diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 69.5 parts is 0.6 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.5 parts, parts by weight are hydroxyethylethylene diamine, the parts by weight of 9.5 parts is 6.The emulsifying agent of 4 parts, parts by weight to be the glacial acetic acid of 6 parts and parts by weight the be defrother of 0.5 part.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 69.5 parts is 0.6 part, parts by weight are 7.5 parts, parts by weight are hydroxyethylethylene diamine, the parts by weight of 9.5 parts is 6.The emulsifying agent of 4 parts, parts by weight are the glacial acetic acid of 6 parts and parts by weight is that the defrother of 0.5 part is as raw material.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 83 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 83 DEG C to stir 19 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 5 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 150 DEG C of insulations 0.5 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 206 DEG C of reactions 2.5 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 94 DEG C to stir 17 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 9.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 69 parts is 0.7 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.7 parts, parts by weight are 9.7 parts, parts by weight are 5.8 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 69 parts is 0.7 part, parts by weight are 7.7 parts, parts by weight are 9.7 parts, parts by weight are 5.8 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 83 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 83 DEG C to stir 22 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 149 DEG C of insulations 1 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 206 DEG C of reactions 2.7 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 108 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 94 DEG C to stir 18 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 10.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 69 parts is 0.7 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.7 parts, parts by weight are 9.7 parts, parts by weight are 5.8 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 69 parts is 0.7 part, parts by weight are 7.7 parts, parts by weight are 9.7 parts, parts by weight are 5.8 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 83 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 83 DEG C to stir 22 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 149 DEG C of insulations 1 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 206 DEG C of reactions 2.7 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 94 DEG C to stir 18 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 11.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 68.5 parts is 0.9 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.9 parts, parts by weight are 9.1 parts, parts by weight are 6.5 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 68.5 parts is 0.9 part, parts by weight are 7.9 parts, parts by weight are 9.1 parts, parts by weight are 6.5 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1840, and emulsifying agent is peregal O-25, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 82 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 82 DEG C to stir 20 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 5 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open nitrogen protection; be warmed up to 149 DEG C of insulations 1 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 205 DEG C of reactions 3 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 95 DEG C to stir 20 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 12.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 68.5 parts is 0.9 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.9 parts, parts by weight are 9.1 parts, parts by weight are 6.5 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is more than 99.5%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 68.5 parts is 0.9 part, parts by weight are 7.9 parts, parts by weight are 9.1 parts, parts by weight are 6.5 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is more than 99.5%.
(2) reaction bulb is heated to 85 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 85 DEG C to stir 20 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 150 DEG C of insulations 0.6 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 205 DEG C of reactions 3 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 95 DEG C to stir 18 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, mass percentage is that the pH value of water solution of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 13.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 69.1 parts is 0.9 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.7 parts, parts by weight are 8.8 parts, parts by weight are 6.4 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 69.1 parts is 0.9 part, parts by weight are 7.7 parts, parts by weight are 8.8 parts, parts by weight are 6.4 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 85 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 85 DEG C to stir 17 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 5 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open nitrogen protection; be warmed up to 150 DEG C of insulations 0.7 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 210 DEG C of reactions 3 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 95 DEG C to stir 19 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, the aqueous ph value of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 14.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 69.3 parts is 0.9 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.6 parts, parts by weight are 8.7 parts, parts by weight are 6.4 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 69.3 parts is 0.9 part, parts by weight are 7.6 parts, parts by weight are 8.7 parts, parts by weight are 6.4 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 83 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 83 DEG C to stir 16 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 3 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 147 DEG C of insulations 1 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 210 DEG C of reactions 2.9 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 95 DEG C to stir 20 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, the pH value of water solution of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 15.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 69.0 parts is 1 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 8.5 parts, parts by weight are 8.0 parts, parts by weight are 6.4 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 69.0 parts is 1 part, parts by weight are 8.5 parts, parts by weight are 8.0 parts, parts by weight are 6.4 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 85 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 85 DEG C to stir 16 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 149 DEG C of insulations 1 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 209 DEG C of reactions 3.0 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 109 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 94 DEG C to stir 20 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, the aqueous ph value of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 16.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 68.5 parts is 1 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 9.0 parts, parts by weight are 8.0 parts, parts by weight are 6.4 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 68.5 parts is 1 part, parts by weight are 9.0 parts, parts by weight are 8.0 parts, parts by weight are 6.4 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 85 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 85 DEG C to stir 17 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 4 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open a little nitrogen protection; be warmed up to 148 DEG C of insulations 0.8 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 209 DEG C of reactions 3.0 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 109 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 94 DEG C to stir 19 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, the aqueous ph value of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 17.
The emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that it be stearic acid, the parts by weight of 68.9 parts is 1 part that the raw material of the cold water instant weak cation soft sheet in the present embodiment comprises parts by weight, parts by weight are 7.6 parts, parts by weight are 8.7 parts, parts by weight are 6.4 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 68.9 parts is 1 part, parts by weight are 7.6 parts, parts by weight are 8.7 parts, parts by weight are 6.4 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.Stearic acid in the present embodiment is stearic acid 1801, and emulsifying agent is emulsifying agent IW, and the purity of diethylenetriamine and hydroxyethylethylene diamine is mass percentage more than 99.0%.
(2) reaction bulb is heated to 83 DEG C, under stirring, the stearic acid in step (1) is added in reaction bulb, keeps temperature 83 DEG C to stir 16 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stirs 3 minutes obtained mixed liquor A.
(3) successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted; open nitrogen protection; be warmed up to 147 DEG C of insulations 1 hour; at this moment the water-band that reaction generates goes out by nitrogen; then 210 DEG C of reactions 2.9 hours are slowly heated to, still by nitrogen protection in this process.Sample analysis surveys acid number, reacts complete, meet the requirements when acid number is less than or equal to 5, continues reaction until acid number meets the requirements when acid number is greater than 5; After meeting the requirements Deng acid number, cool to 110 DEG C of obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 95 DEG C to stir 20 minutes, make it fully dissolve and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, the aqueous ph value of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 18.
The raw material of the cold water instant weak cation soft sheet in the present embodiment comprises the stearic acid that parts by weight are 68 parts, parts by weight are the phosphorous acid of 0.5 part, parts by weight are the diethylenetriamine of 7.0 parts, parts by weight are the hydroxyethylethylene diamine of 8 parts, parts by weight are the emulsifying agent of 5.5 parts, parts by weight to be the glacial acetic acid of 6 parts and parts by weight the be defrother of 0.5 part, wherein, stearic acid can be stearic acid 1801 or stearic acid 1840, emulsifying agent can be peregal O-25 or emulsifying agent IW, the purity of diethylenetriamine and hydroxyethylethylene diamine all can at mass percentage more than 99.0%.
The defrother of the emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that the raw material of the cold water instant weak cation soft sheet in the present invention can comprise stearic acid that parts by weight are 68-72 part, parts by weight are 0.5-1.0 part, parts by weight are 7.0-9.0 part, parts by weight are 8-10 part, parts by weight are 5.5-6.5 part, parts by weight to be the glacial acetic acid of 6-6.5 part and parts by weight be 0.5-0.6 part.
The preparation method of the cold water instant weak cation soft sheet in the present embodiment, is characterized in that: described preparation method in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 68 parts is 0.5 part, parts by weight are 7.0 parts, parts by weight are 8 parts, parts by weight are 5.5 parts, parts by weight are the glacial acetic acid of 6 parts and parts by weight is that the defrother of 0.5 part is as raw material.
(2) reaction bulb is heated to 80 DEG C, under the condition stirred, the stearic acid in step (1) is added in reaction bulb, keep the temperature of 80 DEG C, stir 30 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stir 5 minutes, phosphorous acid and stearic acid are mixed, thus obtained mixed liquor A.
Reaction bulb can be heated to 80-85 DEG C by the present invention, under the condition stirred, the stearic acid in step (1) is added in reaction bulb, the temperature of 80-85 DEG C can be kept, stir 20-30 minute, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, can 3-5 minute be stirred, phosphorous acid and stearic acid are mixed, thus obtained mixed liquor A.
(3) under the condition opening nitrogen protection, first successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted, after diethylenetriamine and hydroxyethylethylene diamine add, be warmed up to 145 DEG C, be incubated 1 hour, at this moment the water-band that reaction generates goes out by nitrogen, is then slowly heated to 200 DEG C, reacts 3 hours; Sample analysis surveys acid number again, when acid number is less than or equal to 5, meets the requirements, reacts complete, when acid number is greater than 5, continues reaction until acid number meets the requirements; After acid number meets the requirements, cool to 105 DEG C, thus obtained mixed liquid B.
The present invention is under the condition opening nitrogen protection, first successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted, after diethylenetriamine and hydroxyethylethylene diamine add, 145-150 DEG C can be warmed up to, insulation 0.5-1 hour, at this moment the water-band that reaction generates goes out by nitrogen, then slowly can be heated to 200-210 DEG C, reaction 2-3 hour; After acid number meets the requirements, can 105-110 DEG C be cooled to, thus obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 90 DEG C, stir 20 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, obtained cold water instant weak cation soft sheet.
Emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B by the present invention successively, can keep temperature 90-95 DEG C, stir 15-20 minute, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mixes.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, the aqueous ph value of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 19.
In the present embodiment, the raw material of cold water instant weak cation soft sheet comprises the stearic acid that parts by weight are 72 parts, parts by weight are the phosphorous acid of 1.0 parts, parts by weight are the diethylenetriamine of 9.0 parts, parts by weight are the hydroxyethylethylene diamine of 10 parts, parts by weight are the emulsifying agent of 6.5 parts, parts by weight to be the glacial acetic acid of 6.5 parts and parts by weight the be defrother of 0.6 part, wherein, stearic acid can be stearic acid 1801 or stearic acid 1840, emulsifying agent can be peregal O-25 or emulsifying agent IW, the purity of diethylenetriamine and hydroxyethylethylene diamine all can at mass percentage more than 99.0%.
In the present embodiment, the preparation method of cold water instant weak cation soft sheet in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 72 parts is 1.0 parts, parts by weight are 9.0 parts, parts by weight are 10 parts, parts by weight are 6.5 parts, parts by weight are the glacial acetic acid of 6.5 parts and parts by weight is that the defrother of 0.6 part is as raw material.
(2) reaction bulb is heated to 85 DEG C, under the condition stirred, the stearic acid in step (1) is added in reaction bulb, keep the temperature of 85 DEG C, stir 20 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stir 3 minutes, phosphorous acid and stearic acid are mixed, thus obtained mixed liquor A.
(3) under the condition opening nitrogen protection, first successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted, after diethylenetriamine and hydroxyethylethylene diamine add, be warmed up to 150 DEG C, be incubated 0.5 hour, at this moment the water-band that reaction generates goes out by nitrogen, is then slowly heated to 210 DEG C, reacts 2 hours; Sample analysis surveys acid number again, when acid number is less than or equal to 5, meets the requirements, reacts complete, when acid number is greater than 5, continues reaction until acid number meets the requirements; After acid number meets the requirements, cool to 110 DEG C, thus obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 95 DEG C, stir 15 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) is obtained, join in cold water and stir lower dissolving rapidly, the aqueous ph value of 5% is at 4.5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 20.
The raw material of the cold water instant weak cation soft sheet in the present embodiment comprises the stearic acid that parts by weight are 70 parts, parts by weight are the phosphorous acid of 0.75 part, parts by weight are the diethylenetriamine of 8 parts, parts by weight are the hydroxyethylethylene diamine of 9 parts, parts by weight are the emulsifying agent of 6 parts, parts by weight to be the glacial acetic acid of 6.25 parts and parts by weight the be defrother of 0.55 part, wherein, stearic acid can be stearic acid 1801 or stearic acid 1840, emulsifying agent can be peregal O-25 or emulsifying agent IW, the purity of diethylenetriamine and hydroxyethylethylene diamine all can at mass percentage more than 99.0%.
In the present embodiment, the preparation method of cold water instant weak cation soft sheet in turn includes the following steps.
(1) emulsifying agent that the hydroxyethylethylene diamine that the diethylenetriamine that the phosphorous acid that to take parts by weight be stearic acid, the parts by weight of 70 parts is 0.75 part, parts by weight are 8 parts, parts by weight are 9 parts, parts by weight are 6 parts, parts by weight are the glacial acetic acid of 6.25 parts and parts by weight is that the defrother of 0.55 part is as raw material.
(2) reaction bulb is heated to 82.5 DEG C, under the condition stirred, the stearic acid in step (1) is added in reaction bulb, keep the temperature of 82.5 DEG C, stir 25 minutes, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stir 4 minutes, phosphorous acid and stearic acid are mixed, thus obtained mixed liquor A.
(3) under the condition opening nitrogen protection, first successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted, after diethylenetriamine and hydroxyethylethylene diamine add, be warmed up to 146 DEG C, be incubated 0.75 hour, at this moment the water-band that reaction generates goes out by nitrogen, is then slowly heated to 205 DEG C, reacts 2.5 hours; Sample analysis surveys acid number again, when acid number is less than or equal to 5, meets the requirements, reacts complete, when acid number is greater than 5, continues reaction until acid number meets the requirements; After acid number meets the requirements, cool to 108 DEG C, thus obtained mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 92.5 DEG C, stir 17.5 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, obtained cold water instant weak cation soft sheet.
The cold water instant weak cation soft sheet that step (4) obtains joins in cold water, and can dissolve rapidly under stirring, mass percentage is that the pH value of water solution of 5% is at 5-6.
The cold water instant weak cation soft sheet obtained in the present embodiment can be dissolved rapidly in cold water, there is low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Although the present invention with embodiment openly as above; but it is also not used to limit protection scope of the present invention; any technical staff being familiar with this technology, not departing from the change and retouching done in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (6)
1. a cold water instant weak cation soft sheet, it is characterized in that: the raw material of this cold water instant weak cation soft sheet comprises the stearic acid that parts by weight are 68-72 part, parts by weight are the phosphorous acid of 0.5-1.0 part, parts by weight are the diethylenetriamine of 7.0-9.0 part, parts by weight are the hydroxyethylethylene diamine of 8-10 part, parts by weight are the emulsifying agent of 5.5-6.5 part, the defrother of parts by weight to be the glacial acetic acid of 6-6.5 part and parts by weight be 0.5-0.6 part, the purity of described diethylenetriamine and hydroxyethylethylene diamine is all at mass percentage more than 99.0%, cold water instant weak cation soft sheet is dissolved into the aqueous solution rapidly in cold water, mass percentage is the pH value of the aqueous solution of 5% is 4.5-6.
2. cold water instant weak cation soft sheet according to claim 1, is characterized in that: described stearic acid is stearic acid 1801 or stearic acid 1840.
3. cold water instant weak cation soft sheet according to claim 1, is characterized in that: described emulsifying agent is peregal O-25 or emulsifying agent IW.
4. a preparation method for cold water instant weak cation soft sheet, is characterized in that: described preparation method in turn includes the following steps:
(1) take stearic acid that parts by weight are 68-72 part, glacial acetic acid that emulsifying agent that hydroxyethylethylene diamine that diethylenetriamine that phosphorous acid that parts by weight are 0.5-1.0 part, parts by weight are 7.0-9.0 part, parts by weight are 8-10 part, parts by weight are 5.5-6.5 part, parts by weight are 6-6.5 part and parts by weight are that the defrother of 0.5-0.6 part is as raw material; The purity of described diethylenetriamine and hydroxyethylethylene diamine is all at mass percentage more than 99.0%;
(2) reaction bulb is heated to 80-85 DEG C, under the condition stirred, the stearic acid in step (1) is added in reaction bulb, keep the temperature of 80-85 DEG C, stir 20-30 minute, stearic acid is dissolved completely, then the phosphorous acid in step (1) is added in reaction bulb, stir 3-5 minute, phosphorous acid and stearic acid are mixed, thus obtained mixed liquor A;
(3) under the condition opening nitrogen protection, first successively the diethylenetriamine in step (1) and hydroxyethylethylene diamine being added in the mixed liquor A of step (2) is slowly reacted, after diethylenetriamine and hydroxyethylethylene diamine add, be warmed up to 145-150 DEG C, insulation 0.5-1 hour, at this moment the water-band that reaction generates goes out by nitrogen, is then heated to 200-210 DEG C, reaction 2-3 hour; Sample analysis surveys acid number again, when acid number is less than or equal to 5, meets the requirements, reacts complete, when acid number is greater than 5, continues reaction until acid number meets the requirements; After acid number meets the requirements, cool to 105-110 DEG C, thus obtained mixed liquid B;
(4) successively emulsifying agent, glacial acetic acid and defrother in step (1) are added in mixed liquid B, keep temperature 90-95 DEG C, stir 15-20 minute, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, obtained cold water instant weak cation soft sheet; Cold water instant weak cation soft sheet is dissolved into the aqueous solution rapidly in cold water, and mass percentage is the pH value of the aqueous solution of 5% is 4.5-6.
5. the preparation method of cold water instant weak cation soft sheet according to claim 4, is characterized in that: described stearic acid is stearic acid 1801 or stearic acid 1840.
6. the preparation method of cold water instant weak cation soft sheet according to claim 4, is characterized in that: described emulsifying agent is peregal O-25 or emulsifying agent IW.
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| CN107523997A (en) * | 2017-08-15 | 2017-12-29 | 广东湛丰精细化工有限公司 | The preparation method of environment-friendly type cation fatty acid softening agent |
| CN109440455A (en) * | 2018-10-08 | 2019-03-08 | 宁波润禾高新材料科技股份有限公司 | A kind of preparation method of the super hydrophilic sheet softening agent of cold water instant dissolving type |
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