CN104592527A - Preparation method of modified silicone oil surfactant for textile - Google Patents
Preparation method of modified silicone oil surfactant for textile Download PDFInfo
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- CN104592527A CN104592527A CN201510068538.0A CN201510068538A CN104592527A CN 104592527 A CN104592527 A CN 104592527A CN 201510068538 A CN201510068538 A CN 201510068538A CN 104592527 A CN104592527 A CN 104592527A
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- silicone oil
- methyl methacrylate
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- toluene
- modified silicone
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000004094 surface-active agent Substances 0.000 title abstract description 12
- 239000004753 textile Substances 0.000 title abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 27
- 239000001257 hydrogen Substances 0.000 claims abstract description 27
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920002614 Polyether block amide Polymers 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 120
- 238000006243 chemical reaction Methods 0.000 claims description 32
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 30
- 239000003921 oil Substances 0.000 claims description 28
- 239000003054 catalyst Substances 0.000 claims description 26
- 150000002431 hydrogen Chemical class 0.000 claims description 26
- 239000013543 active substance Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 15
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 15
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 11
- WZJUBBHODHNQPW-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2$l^{3},4$l^{3},6$l^{3},8$l^{3}-tetraoxatetrasilocane Chemical compound C[Si]1O[Si](C)O[Si](C)O[Si](C)O1 WZJUBBHODHNQPW-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000003729 cation exchange resin Substances 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 230000006837 decompression Effects 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005194 fractionation Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- RSNQKPMXXVDJFG-UHFFFAOYSA-N tetrasiloxane Chemical compound [SiH3]O[SiH2]O[SiH2]O[SiH3] RSNQKPMXXVDJFG-UHFFFAOYSA-N 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 208000027418 Wounds and injury Diseases 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 3
- 208000014674 injury Diseases 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 150000003376 silicon Chemical class 0.000 description 21
- 238000009941 weaving Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- -1 methylmethacrylate modified silicon Chemical class 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000009988 textile finishing Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 239000004900 Hydrophilic Finishing Agent Substances 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 238000007098 aminolysis reaction Methods 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of a modified silicone oil surfactant for textile. The preparation method comprises the following steps: preparing hydrogen-containing silicone oil; preparing methyl methacrylate modified silicone oil; and preparing a polyether amide modified silicone oil surfactant to finally obtain the modified silicone oil surfactant. The preparation method provided by the invention is simple in process steps, easy to control, small in injury to a human body in an operation process, small in pollution, energy-saving, emission-reducing and short in reaction time; the prepared surfactant is good in stability, good in hydrophilcity, easier to self-emulsify and better in emulsion stability, and has the characteristics of low surface tension and high activity.
Description
Technical field
The invention belongs to textile auxiliary agent field, be specifically related to a kind of weaving by the preparation method of modified silicon oil tensio-active agent.
Background technology
In weaving garment industry, organic silicon surfactant is a kind of important auxiliary agent, this is because its raw materials cost is low on the one hand, asepsis environment-protecting, it can be used for the aftertreatment of fabric as softening agent, water-resisting agent, anti-melting finishing composition, static inhibitor, sanitary finish agent, lubricant, defoamer and shrinkproof wrinkle agent on the other hand, can improve elasticity, make fabric have slipping, resistance to crapyness, static resistance, moisture absorption water vapour permeability and soil release performance.
In recent years, the requirement that fast development and people along with science and technology apply organic silicon surfactant is more and more higher, and the organic silicon surfactant of simple function is difficult to practical requirement.In this case, develop multi-functional organic silicon surfactant, modification is again carried out to modified silicon oil, give the important directions that its more more outstanding performance becomes organosilicon material development.Wherein in fabric treating, organic silicon surfactant is a kind of important textile finishing auxiliary agent.By to some fabrics, as cotton, fur, burlap arrange, their feel can be solved coarse, the shortcoming such as ventilative not.
On textile finishing, common quaternary ammonium salt surfactivity antiseptic-germicide belongs to dissolution type, very not washable, and easily lost efficacy and be enriched in human body surface, life-time service is harmful.But quaternary ammonium salt organosilicon cationic tensio-active agent and fiber are in conjunction with for a long time fastening, antibacterial effect is remarkable, belong to non-dissolving type antibacterial finishing agent, to human non-toxic's safety, there is good inhibition to Gram-negative bacteria, yeast and fungi etc., be therefore widely used in the arrangement of towel, carpet, socks, sheet, underwear and operation textile; The features such as Nonionic organosilicon surfactant has high surface, dispersing property is excellent, consumption is few, defoaming capacity is strong and action effect is lasting, are mainly applied in textile industry as defoamer and hydrophilic finishing agent.
Summary of the invention
Technical problem to be solved by this invention is, for the shortcoming that above prior art exists, proposes a kind of weaving and uses the preparation method of modified silicon oil tensio-active agent, this preparation method's processing step is simple, be easy to control, little to the injury of human body in operating process, pollute little, energy-saving and emission-reduction, reaction times is short, and the surfactant stability prepared is good, good hydrophilic property, self-emulsifying is easier and stability of emulsion is better, has low surface tension, highly active feature simultaneously.
The technical scheme that the present invention solves above technical problem is:
Weave by a preparation method for modified silicon oil tensio-active agent, specifically comprise the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soak Zeo-karb 24h with concentrated hydrochloric acid, then use deionized water rinsing 3-5 time, then soak Zeo-karb 24h with deionized water, finally take out Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst cation exchange resin after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 6-8h stirring and heating, catalyst cation exchange resin is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is: 20-25:10-15:0.8-1, catalyst cation exchange resin consumption is the 5-6% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 20-25:22-28:10-13; The consumption of isopropyl alcohol solution of chloroplatinic acid is the 0.005-0.008% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is: 20-25:2-5:6-10; Catalyzer aluminum chloride consumption is the 0.004-0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
The technical scheme that the present invention limits further is:
In the preparation method of aforementioned weaving modified silicon oil tensio-active agent, catalyst cation exchange resin is NKC-9 Zeo-karb.
In the preparation method of aforementioned weaving modified silicon oil tensio-active agent, catalyst particle size is 0.4-0.6mm, and hydrogen ion molality is 6-8mmol/g.
The invention has the beneficial effects as follows: the silicone oil of this amino by polyetheramine of (1) the present invention and band functional group carries out aminolysis reaction and obtains polyetheramides modified silicon oil, give full play to amino modified and polyether-modified two-fold advantage, polyether segment is linked on silicone molecule, improve molecular hydrophylic, emulsification can be carried out without the need to additional emulsifying agent, good emulsion stability, there will not be problems such as " breakdown of emulsion floating oils ".(2) in modifying process of the present invention, primary amino has become secondary amino group after the reaction, and stability is better, and xanthochromia is lower, improves the performance of organosilicon auxiliary agent further.(3) domesticly at present in the synthesis of modified silicon oil, traditional concentrated sulfuric acid catalyst is still adopted, such catalyzer can affect the quality of product, cause silicone oil product ubiquity unstable, trace impurity is many, the shortcomings such as batch wise differences is large, and the strong-acid cation-exchange resin catalyst adopted in the present invention can solve silicone oil product department stable problem, and it is easy to control to synthesis silicone oil reaction process, stable operation, little to human injury, Reaction time shorten, can reclaim and reuse repeatedly, energy-saving and emission-reduction, the advantages such as decreasing pollution.(4) in the present invention, synthesizing methylmethacrylate modified silicon oil adopts containing hydrogen silicone oil and methyl methacrylate to carry out addition reaction to obtain, and step is simple, and be easy to control, the product stability of generation is good.(5) a kind of polyetheramides modified silicon oil of the present invention is a kind of novel organosilicon nonionogenic tenside, wherein siloxanes segment has lipophilicity, polyether segment, amino have wetting ability, better than the wetting ability of general amino-modified silicone oil, self-emulsifying more easily and stability of emulsion more, there is the intrinsic low surface tension of polysiloxane, highly active feature simultaneously.
Embodiment
embodiment 1
The present embodiment provides a kind of and weaves by the preparation method of modified silicon oil tensio-active agent, specifically comprises the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soaking particle diameter with concentrated hydrochloric acid is 0.4mm, hydrogen ion molality is the NKC-9 Zeo-karb 24h of 7mmol/g, then deionized water rinsing is used 3 times, then soak NKC-9 Zeo-karb 24h with deionized water, finally take out NKC-9 Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst n KC-9 Zeo-karb after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 6h stirring and heating, catalyst n KC-9 Zeo-karb is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is 20:12:0.8, catalyst n KC-9 Zeo-karb consumption is 6% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 25:25:12; The consumption of isopropyl alcohol solution of chloroplatinic acid is 0.006% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is 25:4:8; Catalyzer aluminum chloride consumption is 0.004% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
embodiment 2
The present embodiment provides a kind of and weaves by the preparation method of modified silicon oil tensio-active agent, specifically comprises the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soaking particle diameter with concentrated hydrochloric acid is 0.5mm, hydrogen ion molality is the NKC-9 Zeo-karb 24h of 8mmol/g, then deionized water rinsing is used 4 times, then soak NKC-9 Zeo-karb 24h with deionized water, finally take out NKC-9 Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst n KC-9 Zeo-karb after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 8h stirring and heating, catalyst n KC-9 Zeo-karb is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is 25:10:1, catalyst n KC-9 Zeo-karb consumption is 5% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 22:28:10; The consumption of isopropyl alcohol solution of chloroplatinic acid is 0.005% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is 20:5:6; Catalyzer aluminum chloride consumption is 0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
embodiment 3
The present embodiment provides a kind of and weaves by the preparation method of modified silicon oil tensio-active agent, specifically comprises the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soaking particle diameter with concentrated hydrochloric acid is 0.6mm, hydrogen ion molality is the NKC-9 Zeo-karb 24h of 6mmol/g, then deionized water rinsing is used 5 times, then soak NKC-9 Zeo-karb 24h with deionized water, finally take out NKC-9 Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst n KC-9 Zeo-karb after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 7h stirring and heating, catalyst n KC-9 Zeo-karb is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is 22:15:0.9, catalyst n KC-9 Zeo-karb consumption is 5% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 20:22:13; The consumption of isopropyl alcohol solution of chloroplatinic acid is 0.008% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is 23:2:10; Catalyzer aluminum chloride consumption is 0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (3)
1. weave by a preparation method for modified silicon oil tensio-active agent, it is characterized in that, specifically comprise the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soak Zeo-karb 24h with concentrated hydrochloric acid, then use deionized water rinsing 3-5 time, then soak Zeo-karb 24h with deionized water, finally take out Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst cation exchange resin after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 6-8h stirring and heating, catalyst cation exchange resin is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is: 20-25:10-15:0.8-1, catalyst cation exchange resin consumption is the 5-6% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 20-25:22-28:10-13; The consumption of isopropyl alcohol solution of chloroplatinic acid is the 0.005-0.008% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is: 20-25:2-5:6-10; Catalyzer aluminum chloride consumption is the 0.004-0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
2. weave by the preparation method of modified silicon oil tensio-active agent according to claim 1, it is characterized in that: described catalyst cation exchange resin is NKC-9 Zeo-karb.
3. weave according to claim 2 by the preparation method of modified silicon oil tensio-active agent, it is characterized in that: described catalyst particle size is 0.4-0.6mm, hydrogen ion molality is 6-8mmol/g.
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| CN115160573A (en) * | 2022-07-15 | 2022-10-11 | 安徽信息工程学院 | A kind of preparation method of hydrocarbon carboxyl modified silicone oil emulsion |
| CN119061701A (en) * | 2024-11-01 | 2024-12-03 | 桐乡市恒隆化工有限公司 | A surfactant for fabric treatment capable of withstanding low temperatures and a preparation method thereof |
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