CN103352367A - 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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- CN103352367A CN103352367A CN2013102118624A CN201310211862A CN103352367A CN 103352367 A CN103352367 A CN 103352367A CN 2013102118624 A CN2013102118624 A CN 2013102118624A CN 201310211862 A CN201310211862 A CN 201310211862A CN 103352367 A CN103352367 A CN 103352367A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 214
- 150000001768 cations Chemical class 0.000 title claims abstract description 133
- 238000002360 preparation method Methods 0.000 title claims abstract description 61
- 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 147
- 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
- 238000005303 weighing Methods 0.000 claims abstract description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 155
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 126
- 238000003756 stirring Methods 0.000 claims description 122
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 claims description 119
- 239000000203 mixture Substances 0.000 claims description 83
- 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
- 238000004458 analytical method Methods 0.000 claims description 22
- 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
- 239000004744 fabric Substances 0.000 description 29
- 229920000742 Cotton Polymers 0.000 description 24
- 238000009434 installation Methods 0.000 description 22
- 238000009413 insulation Methods 0.000 description 17
- 239000000243 solution Substances 0.000 description 15
- 238000004043 dyeing Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- -1 cation fatty acid Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 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
- 239000004753 textile Substances 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
- 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
- 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 dissolving weak cation flexible sheet and preparation method thereof, the softener mainly as textile printing and dyeing processing can carry out soft finish to fiber, fabric.
Background technology
Textile fiber yarn or fabric generally all need be removed the commensals such as the contained wax of natural fabric and grease through scouringing and bleaching pre-treatment, cause fabric to produce more coarse feel.In order to make fabric have lasting, soft feel, generally all require after dyeing, to carry out soft treatment.Using more widely, surfactant mainly is cationic softener, cheap CATION flexible sheet occupies very large ratio in softener, printing and dyeing mill changes into emulsion to film and uses, but these flexible sheets all will could dissolve in 70-80 ℃ hot water, the material time is long, waste energy, and the xanthochromia degree is high, flatness is poor.
The relatively better gentle sheet of CATION of some performances is also arranged at present, as open day be on 06 09th, 2010, publication number is in the Chinese patent of CN101725043A, a kind of low-temperature instant flexible sheets and preparation method thereof is disclosed, this low-temperature instant flexible sheets is made by 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 be at dissolution in low temperature, low-yellowing, but flatness is slightly poor, and the color that the control of manufacture process conditional is bad is dark.And for example disclosed day on December 14th, 2011, publication number is in the Chinese patent of CN102277739A, a kind of preparation method of weak cation fatty acid softening agent is disclosed, this preparation method may further comprise the steps: fixed oil is heated to fusing, after adding antioxidant diethylenetriamine is added above-mentioned fused solution, then add successively hydroxyethylethylene diamine, diethanol amine, carry out amidatioon condensation reaction and ester exchange reaction after the intensification; In the product of described amide condensed reaction, add alkylating reagent acetic acid and formic acid, carry out alkylation reaction, then cool off the blowing section, this softener xanthochromia of sheet softener is low, good hand touch although make, but solution temperature is high, and the material time is long, loses time and the energy.
Also there be not now a kind of can in cold water, the dissolving rapidly, low-yellowing, soft smooth, biological degradability is good, is applicable to cold water instant dissolving weak cation flexible 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 the prior art, can in cold water, dissolve rapidly and provide a kind of, low-yellowing is soft smooth, biological degradability is good, is applicable to cold water instant dissolving weak cation flexible sheet of cotton fiber and BLENDED FABRIC soft finish thereof and preparation method thereof.
The present invention addresses the above problem the technical scheme that adopts: the characteristics of this cold water instant dissolving weak cation flexible sheet are: the raw material of this cold water instant dissolving weak cation flexible sheet comprises that parts by weight are the stearic acid of 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, parts by weight are that glacial acetic acid and the parts by weight of 6-6.5 part are the defrother of 0.5-0.6 part.Thus so that the cold water instant dissolving weak cation flexible sheet among the present invention can be in cold water rapidly dissolving, have low-yellowing, soft smooth, characteristics that biological degradability is good, be applicable to the soft finish of cotton fiber and BLENDED FABRIC thereof.Cold water instant dissolving weak cation flexible sheet joins in the cold water, under agitation can dissolve rapidly, and the quality percentage composition is that the pH value of 5% the aqueous solution 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 the quality percentage composition more than 99.0%.
The preparation method's of cold water instant dissolving weak cation flexible sheet characteristics are among the present invention: described preparation method in turn includes the following steps:
(1) takes by weighing defrother that stearic acid that parts by weight are 68-72 part, phosphorous acid that parts by weight are 0.5-1.0 part, diethylenetriamine that parts by weight are 7.0-9.0 part, hydroxyethylethylene diamine that parts by weight are 8-10 part, emulsifying agent that parts by weight are 5.5-6.5 part, glacial acetic acid that parts by weight are 6-6.5 part and parts by weight are 0.5-0.6 part as raw material;
(2) reaction bulb is heated to 80-85 ℃, under the condition that stirs, the stearic acid in the step (1) is added in the reaction bulb, keep 80-85 ℃ temperature, stirred 20-30 minute, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirred 3-5 minute, so that phosphorous acid and stearic acid mix, thereby make mixed liquor A;
(3) opening under the condition of nitrogen protection, to react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively first, when diethylenetriamine and hydroxyethylethylene diamine add complete after, be warmed up to 145-150 ℃, be incubated 0.5-1 hour, at this moment nitrogen will react the water that generates and take out of, then be heated to 200-210 ℃, react 2-3 hour; Sample analysis is surveyed acid number again, when acid number less than or equal to 5 the time, meet the requirements, react complete, when acid number greater than 5 the time, continue to react until acid number meets the requirements; After acid number meets the requirements, cool to 105-110 ℃, thereby make mixed liquid B;
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 90-95 ℃ of temperature, stirred 15-20 minute, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
So that the preparation method of the cold water instant dissolving weak cation flexible sheet among the present invention is simple, processing ease does not need special installation thus, 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 the quality percentage composition more than 99.0%.
The present invention compared with prior art has the following advantages and effect: cold water instant dissolving weak cation flexible sheet can dissolve rapidly in cold water, has low-yellowing, and soft smooth, biological degradability is good, is applicable to cotton fiber and BLENDED FABRIC soft finish thereof.
The preparation method of cold water instant dissolving weak cation flexible sheet is simple among the present invention, and processing ease does not need special installation, and reaction condition is gentle, and production cost is low.
The specific embodiment
The present invention is described in further detail below by embodiment, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 70.5 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The raw material of cold water instant dissolving weak cation flexible sheet can comprise that parts by weight are that the stearic acid of 68-72 part, the phosphorous acid that parts by weight are 0.5-1.0 part, the diethylenetriamine that parts by weight are 7.0-9.0 part, the hydroxyethylethylene diamine that parts by weight are 8-10 part, the emulsifying agent that parts by weight are 5.5-6.5 part, glacial acetic acid and the parts by weight that parts by weight are 6-6.5 part are the defrother of 0.5-0.6 part among the present invention.Wherein, what stearic acid can be in stearic acid 1801 and the stearic acid 1840 is a kind of, and what emulsifying agent can be among peregal O-25 and the emulsifying agent IW is a kind of.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 70.5 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.5 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 80 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 80 ℃ of temperature to stir 20 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 3 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; stir in the course of reaction; and open a little nitrogen and protect; be warmed up to 145 ℃ of insulations 0.6 hour; at this moment nitrogen will react the water that generates and take out of; then be heated to 200 ℃ of reactions 2 hours, remain unchanged by nitrogen protection in this course of reaction.Sample analysis is surveyed acid number, when acid number less than or equal to 5 the time, react complete, meet the requirements; When acid number greater than 5 the time, continue reaction, until acid number meets the requirements; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.Because stearic acid and amine exothermic heat of reaction, so in diethylenetriamine and the hydroxyethylethylene diamine needs mixed liquor A that is added to step (2) slowly.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 90 ℃ of temperature to stir 15 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.Composition was consistent before and after section referred to stir in the slicing processes and makes the sheet softener under the stirring among the present invention, and this belongs to common practise.
The cold water instant dissolving weak cation flexible sheet that the present embodiment step (4) makes joins in the cold water, just can dissolve rapidly under stirring, and the quality percentage composition is 5% the aqueous solution after the dissolving, and its pH value is at 5-6.Cold water instant dissolving weak cation flexible sheet among the present invention joins in the cold water and can dissolve rapidly, and placing the 950ml temperature such as the 50g flexible sheet is 30 ℃ water, stirs a minutes with glass bar and just can dissolve fully by hand.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 2.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 71 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7.1 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.4 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing the defrother that parts by weight are 71 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7.1 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.4 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 81 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 81 ℃ of temperature to stir 21 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 3 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 146 ℃ of insulations 0.7 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 200 ℃ of reactions 2 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 108 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 92 ℃ of temperature to stir 16 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that the present embodiment step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 3.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 71 parts stearic acid, phosphorous acid that parts by weight are 0.6 part, parts by weight are 7.2 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.7 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.4 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 71 parts stearic acid, phosphorous acid that parts by weight are 0.6 part, parts by weight are 7.2 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.7 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.4 parts and parts by weight are 0.5 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 82 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 82 ℃ of temperature to stir 22 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 147 ℃ of insulations 0.7 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 201 ℃ of reactions 2.1 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 93 ℃ of temperature to stir 16 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 4.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 71.4 parts stearic acid, phosphorous acid that parts by weight are 0.6 part, parts by weight are 8 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8 parts, emulsifying agent that parts by weight are 5.5 parts, glacial acetic acid that parts by weight are 6 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 71.4 parts stearic acid, phosphorous acid that parts by weight are 0.6 part, parts by weight are 8 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8 parts, emulsifying agent that parts by weight are 5.5 parts, glacial acetic acid that parts by weight are 6 parts and parts by weight are 0.5 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 83 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 83 ℃ of temperature to stir 22 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 148 ℃ of insulations 0.8 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 202 ℃ of reactions 2.5 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to again 109 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 99 ℃ of temperature to stir 18 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 5.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 70.5 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 70.5 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.5 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 85 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 85 ℃ of temperature to stir 20 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 3 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 145 ℃ of insulations 0.6 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 205 ℃ of reactions 2.3 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 109 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 90 ℃ of temperature to stir 15 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 6.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 70.5 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 70.5 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.5 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 84 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 84 ℃ of temperature to stir 25 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 5 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 148 ℃ of insulations 0.8 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 204 ℃ of reactions 2.6 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to again 107 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 93 ℃ of temperature to stir 18 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 7.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 69.5 parts stearic acid, phosphorous acid that parts by weight are 0.6 part, parts by weight are 7.5 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.5 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 69.5 parts stearic acid, phosphorous acid that parts by weight are 0.6 part, parts by weight are 7.5 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.5 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6 parts and parts by weight are 0.5 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 85 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 85 ℃ of temperature to stir 21 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 146 ℃ of insulations 0.9 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 207 ℃ of reactions 2.4 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, when acid number less than or equal to 5 the time, meet the requirements, react complete, when acid number greater than 5 the time, continue to react, until acid number meets the requirements; After meeting the requirements Deng acid number, cool to 105 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 95 ℃ of temperature to stir 17 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 8.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises that parts by weight are that 69.5 parts stearic acid, the phosphorous acid that parts by weight are 0.6 part, the diethylenetriamine that parts by weight are 7.5 parts, hydroxyethylethylene diamine, the parts by weight that parts by weight are 9.5 parts are 6.4 parts emulsifying agent, parts by weight are the defrother that 6 parts glacial acetic acid and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) taking by weighing parts by weight is that 69.5 parts stearic acid, the phosphorous acid that parts by weight are 0.6 part, the diethylenetriamine that parts by weight are 7.5 parts, hydroxyethylethylene diamine, the parts by weight that parts by weight are 9.5 parts are 6.4 parts emulsifying agent, parts by weight be 6 parts glacial acetic acid and parts by weight be 0.5 part defrother 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 83 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 83 ℃ of temperature to stir 19 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 5 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 150 ℃ of insulations 0.5 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 206 ℃ of reactions 2.5 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 94 ℃ of temperature to stir 17 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 9.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 69 parts stearic acid, phosphorous acid that parts by weight are 0.7 part, parts by weight are 7.7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.7 parts, emulsifying agent that parts by weight are 5.8 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 69 parts stearic acid, phosphorous acid that parts by weight are 0.7 part, parts by weight are 7.7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.7 parts, emulsifying agent that parts by weight are 5.8 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 83 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 83 ℃ of temperature to stir 22 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 149 ℃ of insulations 1 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 206 ℃ of reactions 2.7 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 108 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 94 ℃ of temperature to stir 18 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 10.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 69 parts stearic acid, phosphorous acid that parts by weight are 0.7 part, parts by weight are 7.7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.7 parts, emulsifying agent that parts by weight are 5.8 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 69 parts stearic acid, phosphorous acid that parts by weight are 0.7 part, parts by weight are 7.7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.7 parts, emulsifying agent that parts by weight are 5.8 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 83 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 83 ℃ of temperature to stir 22 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 149 ℃ of insulations 1 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 206 ℃ of reactions 2.7 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 94 ℃ of temperature to stir 18 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 11.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 68.5 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.9 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.1 parts, emulsifying agent that parts by weight are 6.5 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 68.5 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.9 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.1 parts, emulsifying agent that parts by weight are 6.5 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 82 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 82 ℃ of temperature to stir 20 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 5 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open nitrogen protection; be warmed up to 149 ℃ of insulations 1 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 205 ℃ of reactions 3 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 95 ℃ of temperature to stir 20 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 12.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 68.5 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.9 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.1 parts, emulsifying agent that parts by weight are 6.5 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 68.5 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.9 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9.1 parts, emulsifying agent that parts by weight are 6.5 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 85 ℃ of temperature to stir 20 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 150 ℃ of insulations 0.6 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 205 ℃ of reactions 3 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 95 ℃ of temperature to stir 18 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water and to stir lower rapidly dissolving, and the quality percentage composition is that 5% pH value of water solution is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 13.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 69.1 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.8 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 69.1 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.7 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.8 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 85 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 85 ℃ of temperature to stir 17 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 5 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open nitrogen protection; be warmed up to 150 ℃ of insulations 0.7 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 210 ℃ of reactions 3 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 95 ℃ of temperature to stir 19 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins and stirs lower rapidly dissolving in the cold water, and 5% aqueous ph value is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 14.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 69.3 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.6 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.7 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 69.3 parts stearic acid, phosphorous acid that parts by weight are 0.9 part, parts by weight are 7.6 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.7 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 83 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 83 ℃ of temperature to stir 16 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 3 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 147 ℃ of insulations 1 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 210 ℃ of reactions 2.9 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 95 ℃ of temperature to stir 20 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins and stirs lower rapidly dissolving in the cold water, and 5% pH value of water solution is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 15.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 69.0 parts stearic acid, phosphorous acid that parts by weight are 1 part, parts by weight are 8.5 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.0 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 69.0 parts stearic acid, phosphorous acid that parts by weight are 1 part, parts by weight are 8.5 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.0 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 85 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 85 ℃ of temperature to stir 16 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 149 ℃ of insulations 1 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 209 ℃ of reactions 3.0 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 109 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 94 ℃ of temperature to stir 20 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins and stirs lower rapidly dissolving in the cold water, and 5% aqueous ph value is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 16.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 68.5 parts stearic acid, phosphorous acid that parts by weight are 1 part, parts by weight are 9.0 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.0 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 68.5 parts stearic acid, phosphorous acid that parts by weight are 1 part, parts by weight are 9.0 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.0 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 85 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 85 ℃ of temperature to stir 17 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 4 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open a little nitrogen protection; be warmed up to 148 ℃ of insulations 0.8 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 209 ℃ of reactions 3.0 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 109 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 94 ℃ of temperature to stir 19 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins and stirs lower rapidly dissolving in the cold water, and 5% aqueous ph value is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 17.
The raw material of the cold water instant dissolving weak cation flexible sheet in the present embodiment comprises the defrother that parts by weight are 68.9 parts stearic acid, phosphorous acid that parts by weight are 1 part, parts by weight are 7.6 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.7 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 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 the quality percentage composition more than 99.0%.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 68.9 parts stearic acid, phosphorous acid that parts by weight are 1 part, parts by weight are 7.6 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8.7 parts, emulsifying agent that parts by weight are 6.4 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part 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 the quality percentage composition more than 99.0%.
(2) reaction bulb is heated to 83 ℃, under stirring the stearic acid in the step (1) is added in the reaction bulb, keeps 83 ℃ of temperature to stir 16 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirs and made mixed liquor A in 3 minutes.
(3) will react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively; open nitrogen protection; be warmed up to 147 ℃ of insulations 1 hour; at this moment nitrogen will react the water that generates and take out of; then slowly be heated to 210 ℃ of reactions 2.9 hours, remain unchanged by nitrogen protection in this process.Sample analysis is surveyed acid number, and is complete when acid number reaction less than or equal to 5 time, meets the requirements, when acid number continues reaction until acid number meets the requirements greater than 5 the time; After meeting the requirements Deng acid number, cool to 110 ℃ and make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 95 ℃ of temperature to stir 20 minutes, it is fully dissolved mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins and stirs lower rapidly dissolving in the cold water, and 5% aqueous ph value is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the 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 dissolving weak cation flexible sheet in the present embodiment comprises that parts by weight are 68 parts stearic acid, parts by weight are 0.5 part phosphorous acid, parts by weight are 7.0 parts diethylenetriamine, parts by weight are 8 parts hydroxyethylethylene diamine, parts by weight are 5.5 parts emulsifying agent, parts by weight are the defrother that 6 parts glacial acetic acid and parts by weight are 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, and the purity of diethylenetriamine and hydroxyethylethylene diamine all can be at the quality percentage composition more than 99.0%.
The raw material of the cold water instant dissolving weak cation flexible sheet among the present invention can comprise that parts by weight are that the stearic acid of 68-72 part, the phosphorous acid that parts by weight are 0.5-1.0 part, the diethylenetriamine that parts by weight are 7.0-9.0 part, the hydroxyethylethylene diamine that parts by weight are 8-10 part, the emulsifying agent that parts by weight are 5.5-6.5 part, glacial acetic acid and the parts by weight that parts by weight are 6-6.5 part are the defrother of 0.5-0.6 part.
The preparation method of the cold water instant dissolving weak cation flexible sheet in the present embodiment, it is characterized in that: described preparation method in turn includes the following steps.
(1) takes by weighing defrother that parts by weight are 68 parts stearic acid, phosphorous acid that parts by weight are 0.5 part, parts by weight are 7.0 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 8 parts, emulsifying agent that parts by weight are 5.5 parts, glacial acetic acid that parts by weight are 6 parts and parts by weight are 0.5 part as raw material.
(2) reaction bulb is heated to 80 ℃, under the condition that stirs, the stearic acid in the step (1) is added in the reaction bulb, keep 80 ℃ temperature, stirred 30 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirred 5 minutes, so that phosphorous acid and stearic acid mix, thereby make mixed liquor A.
The present invention can be heated to reaction bulb 80-85 ℃, under the condition that stirs, the stearic acid in the step (1) is added in the reaction bulb, can keep 80-85 ℃ temperature, stirred 20-30 minute, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, can stir 3-5 minute, so that phosphorous acid and stearic acid mix, thereby make mixed liquor A.
(3) opening under the condition of nitrogen protection, to react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively first, when diethylenetriamine and hydroxyethylethylene diamine add complete after, be warmed up to 145 ℃, be incubated 1 hour, at this moment nitrogen will react the water that generates and take out of, then slowly be heated to 200 ℃, react 3 hours; Sample analysis is surveyed acid number again, when acid number less than or equal to 5 the time, meet the requirements, react complete, when acid number greater than 5 the time, continue to react until acid number meets the requirements; After acid number meets the requirements, cool to 105 ℃, thereby make mixed liquid B.
The present invention is opening under the condition of nitrogen protection, to react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively first, when diethylenetriamine and hydroxyethylethylene diamine add complete after, can be warmed up to 145-150 ℃, be incubated 0.5-1 hour, at this moment nitrogen will react the water that generates and take out of, then can slowly be heated to 200-210 ℃, react 2-3 hour; After acid number meets the requirements, can cool to 105-110 ℃, thereby make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 90 ℃ of temperature, stirred 20 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The present invention is added to emulsifying agent, glacial acetic acid and defrother in the step (1) in the mixed liquid B successively, can keep temperature 90-95 ℃, stirs 15-20 minute, emulsifying agent, glacial acetic acid and defrother is fully dissolved, and mix.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins and stirs lower rapidly dissolving in the cold water, and 5% aqueous ph value is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the preparation method is simple, processing ease, do not need special installation, reaction condition is gentle, and production cost is low.
Embodiment 19.
The raw material of cold water instant dissolving weak cation flexible sheet comprises that parts by weight are 72 parts stearic acid in the present embodiment, parts by weight are 1.0 parts phosphorous acid, parts by weight are 9.0 parts diethylenetriamine, parts by weight are 10 parts hydroxyethylethylene diamine, parts by weight are 6.5 parts emulsifying agent, parts by weight are the defrother that 6.5 parts glacial acetic acid and parts by weight are 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, and the purity of diethylenetriamine and hydroxyethylethylene diamine all can be at the quality percentage composition more than 99.0%.
The preparation method of cold water instant dissolving weak cation flexible sheet in turn includes the following steps in the present embodiment.
(1) takes by weighing defrother that parts by weight are 72 parts stearic acid, phosphorous acid that parts by weight are 1.0 parts, parts by weight are 9.0 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 10 parts, emulsifying agent that parts by weight are 6.5 parts, glacial acetic acid that parts by weight are 6.5 parts and parts by weight are 0.6 part as raw material.
(2) reaction bulb is heated to 85 ℃, under the condition that stirs, the stearic acid in the step (1) is added in the reaction bulb, keep 85 ℃ temperature, stirred 20 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirred 3 minutes, so that phosphorous acid and stearic acid mix, thereby make mixed liquor A.
(3) opening under the condition of nitrogen protection, to react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively first, when diethylenetriamine and hydroxyethylethylene diamine add complete after, be warmed up to 150 ℃, be incubated 0.5 hour, at this moment nitrogen will react the water that generates and take out of, then slowly be heated to 210 ℃, react 2 hours; Sample analysis is surveyed acid number again, when acid number less than or equal to 5 the time, meet the requirements, react complete, when acid number greater than 5 the time, continue to react until acid number meets the requirements; After acid number meets the requirements, cool to 110 ℃, thereby make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 95 ℃ of temperature, stirred 15 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins and stirs lower rapidly dissolving in the cold water, and 5% aqueous ph value is at 4.5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the 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 dissolving weak cation flexible sheet in the present embodiment comprises that parts by weight are 70 parts stearic acid, parts by weight are 0.75 part phosphorous acid, parts by weight are 8 parts diethylenetriamine, parts by weight are 9 parts hydroxyethylethylene diamine, parts by weight are 6 parts emulsifying agent, parts by weight are the defrother that 6.25 parts glacial acetic acid and parts by weight are 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, and the purity of diethylenetriamine and hydroxyethylethylene diamine all can be at the quality percentage composition more than 99.0%.
The preparation method of cold water instant dissolving weak cation flexible sheet in turn includes the following steps in the present embodiment.
(1) takes by weighing defrother that parts by weight are 70 parts stearic acid, phosphorous acid that parts by weight are 0.75 part, parts by weight are 8 parts diethylenetriamine, hydroxyethylethylene diamine that parts by weight are 9 parts, emulsifying agent that parts by weight are 6 parts, glacial acetic acid that parts by weight are 6.25 parts and parts by weight are 0.55 part as raw material.
(2) reaction bulb is heated to 82.5 ℃, under the condition that stirs, the stearic acid in the step (1) is added in the reaction bulb, keep 82.5 ℃ temperature, stirred 25 minutes, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirred 4 minutes, so that phosphorous acid and stearic acid mix, thereby make mixed liquor A.
(3) opening under the condition of nitrogen protection, to react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively first, when diethylenetriamine and hydroxyethylethylene diamine add complete after, be warmed up to 146 ℃, be incubated 0.75 hour, at this moment nitrogen will react the water that generates and take out of, then slowly be heated to 205 ℃, react 2.5 hours; Sample analysis is surveyed acid number again, when acid number less than or equal to 5 the time, meet the requirements, react complete, when acid number greater than 5 the time, continue to react until acid number meets the requirements; After acid number meets the requirements, cool to 108 ℃, thereby make mixed liquid B.
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 92.5 ℃ of temperature, stirred 17.5 minutes, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
The cold water instant dissolving weak cation flexible sheet that step (4) makes joins in the cold water, can dissolve rapidly under stirring, and the quality percentage composition is that 5% pH value of water solution is at 5-6.
The cold water instant dissolving weak cation flexible sheet that obtains in the present embodiment can dissolve rapidly in cold water, has low-yellowing, soft smooth, biological degradability is good, be applicable to cotton fiber and BLENDED FABRIC soft finish thereof, and the 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 not to limit protection scope of the present invention; any technical staff who is familiar with this technology not breaking away from change and the retouching of doing in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (8)
1. cold water instant dissolving weak cation flexible sheet is characterized in that: the raw material of this cold water instant dissolving weak cation flexible sheet comprises that parts by weight are that the stearic acid of 68-72 part, the phosphorous acid that parts by weight are 0.5-1.0 part, the diethylenetriamine that parts by weight are 7.0-9.0 part, the hydroxyethylethylene diamine that parts by weight are 8-10 part, the emulsifying agent that parts by weight are 5.5-6.5 part, glacial acetic acid and the parts by weight that parts by weight are 6-6.5 part are the defrother of 0.5-0.6 part.
2. cold water instant dissolving weak cation flexible sheet according to claim 1, it is characterized in that: described stearic acid is stearic acid 1801 or stearic acid 1840.
3. cold water instant dissolving weak cation flexible sheet according to claim 1, it is characterized in that: described emulsifying agent is peregal O-25 or emulsifying agent IW.
4. cold water instant dissolving weak cation flexible sheet according to claim 1 is characterized in that: the purity of described diethylenetriamine and hydroxyethylethylene diamine is all at the quality percentage composition more than 99.0%.
5. the preparation method of a cold water instant dissolving weak cation flexible sheet, it is characterized in that: described preparation method in turn includes the following steps:
(1) takes by weighing defrother that stearic acid that parts by weight are 68-72 part, phosphorous acid that parts by weight are 0.5-1.0 part, diethylenetriamine that parts by weight are 7.0-9.0 part, hydroxyethylethylene diamine that parts by weight are 8-10 part, emulsifying agent that parts by weight are 5.5-6.5 part, glacial acetic acid that parts by weight are 6-6.5 part and parts by weight are 0.5-0.6 part as raw material;
(2) reaction bulb is heated to 80-85 ℃, under the condition that stirs, the stearic acid in the step (1) is added in the reaction bulb, keep 80-85 ℃ temperature, stirred 20-30 minute, stearic acid is dissolved fully, then the phosphorous acid in the step (1) is added in the reaction bulb, stirred 3-5 minute, so that phosphorous acid and stearic acid mix, thereby make mixed liquor A;
(3) opening under the condition of nitrogen protection, to react in the diethylenetriamine in the step (1) and the hydroxyethylethylene diamine mixed liquor A that is added to step (2) slowly successively first, when diethylenetriamine and hydroxyethylethylene diamine add complete after, be warmed up to 145-150 ℃, be incubated 0.5-1 hour, at this moment nitrogen will react the water that generates and take out of, then be heated to 200-210 ℃, react 2-3 hour; Sample analysis is surveyed acid number again, when acid number less than or equal to 5 the time, meet the requirements, react complete, when acid number greater than 5 the time, continue to react until acid number meets the requirements; After acid number meets the requirements, cool to 105-110 ℃, thereby make mixed liquid B;
(4) successively emulsifying agent, glacial acetic acid and defrother in the step (1) are added in the mixed liquid B, keep 90-95 ℃ of temperature, stirred 15-20 minute, emulsifying agent, glacial acetic acid and defrother are fully dissolved, and mix, stir lower section, make cold water instant dissolving weak cation flexible sheet.
6. the preparation method of cold water instant dissolving weak cation flexible sheet according to claim 5, it is characterized in that: described stearic acid is stearic acid 1801 or stearic acid 1840.
7. the preparation method of cold water instant dissolving weak cation flexible sheet according to claim 5, it is characterized in that: described emulsifying agent is peregal O-25 or emulsifying agent IW.
8. the preparation method of cold water instant dissolving weak cation flexible sheet according to claim 5 is characterized in that: the purity of described diethylenetriamine and hydroxyethylethylene diamine is all at the quality percentage composition more than 99.0%.
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| CN106676892A (en) * | 2016-12-30 | 2017-05-17 | 广东德美精细化工股份有限公司 | Preparation method of novel softener highly resistant to phenolic yellowing |
| 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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| 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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