CN107881787A - A kind of preparation method of high washable antistatic additive - Google Patents
A kind of preparation method of high washable antistatic additive Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/507—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
Abstract
The invention discloses a kind of preparation method of high washable antistatic additive, belong to electrostatic agent preparing technical field.The present invention forms self-control copolymer using polyester and polyethers copolyreaction,Washability is from polyester segment and the film forming of whole polymer,Molecular weight is bigger,Film more strong and washability is better,Polyester segment is the more,And washability is better,After polyacrylate dispersion moisture evaporation,One layer of insoluble epithelium is formed in anti-static fabric fiber surface,Initiator and cross-linking monomer are added again,Continuously add Ludox,And hydrophobically modified is carried out to Ludox with hydrophobic substance,Caused silanol with the remaining hydroxyl of silica particle surface continues that intermolecular dehydration occurs after hydrolysis,Finally it is immersed in and is mixed by sericin powder and citric acid in self-control solution,Because sericin powder is anchored on anti-static fabric fiber by ester bond,Washing makes its difficult for drop-off repeatedly,Further improve the washability of antistatic additive,It is with a wide range of applications.
Description
Technical field
The invention discloses a kind of preparation method of high washable antistatic additive, belong to antistatic additive preparing technical field.
Background technology
Terylene is an important kind in synthetic fibers, is the trade name of China's polyester fiber.It is to benzene two with essence
Formic acid or dimethyl terephthalate (DMT) and ethylene glycol be raw material through esterification or ester exchange with it is into fine high poly- prepared by polycondensation reaction
Thing polyethylene terephthalate, through fiber made of spinning and post processing.
Due to the electrostatic phenomenon of textile fabric, when textile process and consumer are applied, the problem of various is brought.
For example, in textile fabric manufacture processing, by the shredding of fiber, comb, the package build and anti-fluffing and anti-pilling of yarn and anti-
Dirt brings many difficulties.Caused due to electrostatic interaction and inhale dust and stain, made between clothes, that clothes and human body produce winding is existing
As, and when walking about on carpet or being rubbed on drapery, have electric shock effect.People on chemical fibre carpet when walking, people
Body will take 3000~5000V electrostatic, when relative humidity is low, up to 5000~18000V.The electrostatic phenomenon of textile
The normal work of meeting interference calculation machine and other sensitive electronic instruments, also, can cause combustibility when a large amount of electric charges are released
The burning of gas and dust.So it is necessary to carry out antistatic finish to textile.
Terylene is a kind of widely used synthetic fibers, and still, hydrophilic radical is less in Structure of PET Fiber, hygroscopicity
Difference, electrostatic easily being produced, this is resulted in during taking, and dacron can not only adsorb the dust in air, and easily
Produce shock phenomenon.Factory commonly uses antistatic additive and antistatic treatment is done to dacron in process of production, but more difficult acquisition is resistance to
Long antistatic effect.Therefore, invent a kind of high washable antistatic additive has positive effect to antistatic additive preparing technical field.
The content of the invention
The technical problems to be solved by the invention:It can assign fabric good antistatic for current common antistatic additive
Property, but the washability of its antistatic finish effect is poor, it is impossible to the defects of meeting anti-static fabric life requirement, there is provided
A kind of preparation method of high washable antistatic additive.
In order to solve the above technical problems, the present invention is using technical scheme as described below:
A kind of preparation method of high washable antistatic additive, it is characterised in that specifically preparation process is:
(1)Sericin powder and citric acid are mixed and stirred in the beaker for pouring into the deionized water with 3~5 times of sericin powder quality, is stirred
The sodium hypophosphite of citric acid quality 40% is added after mixing, continues to mix, obtains making solution by oneself;
(2)Weigh 80~90g methanol Ludox to pour into three-necked flask, three-necked flask is put into water-bath and stirred, then to three
10~12mL MTMSs and 6~8mL MethylethoxylsiliconFluid Fluids are added in mouth flask, continues insulation reaction, is continued
After adding the mixing of 70~90g propylene glycol methyl ether acetates into three-necked flask, obtain reacting glue, reaction glue is transferred to rotation
Turn evaporator for decompression distillation, remove methanol, obtain modified from preparing silicon collosol;
(3)Count in parts by weight, weigh dimethyl terephthalate (DMT) respectively, polyethylene glycol mixing is placed in equipped with agitator, condensation
Stirred in the four-hole boiling flask of pipe and thermometer, zinc acetate and antimony oxide are added into four-hole boiling flask, under the protection of nitrogen
Mix, and heat temperature raising, obtain being esterified material, continue under the protection of nitrogen, zinc acetate, Asia are added into esterification material
Triphenyl phosphate hybrid reaction, continue heat temperature raising, treat no gas effusion, Temperature fall, discharging, obtain making copolymer by oneself;
(4)Count in parts by weight, weigh self-control copolymer respectively, modified mixed from preparing silicon collosol and deionized water is placed in mixer
Middle stirring, then polyacrylate dispersion, potassium peroxydisulfate and itaconic acid are added, continue to mix, naturally cool to room temperature, obtain
Antistatic base substrate, antistatic base substrate is added in self-control solution and soaked, is put into baking oven and dries after immersion, grinding discharging, i.e.,
High washable antistatic additive can be made.
Step(1)Described sericin powder and the same-size ratio of citric acid, mixing time are 6~8min, continue mixing time and are
20~30min.
Step(2)Described whipping temp is 45~65 DEG C, and mixing time is 16~20min, MethylethoxylsiliconFluid Fluid
Mass fraction is 2%, and the reaction time is 45~60min, and continuation mixing time is 10~12min, be evaporated under reduced pressure the time be 20~
30min。
Step(3)Described meter in parts by weight, weigh respectively 10~12 parts of dimethyl terephthalate (DMT)s, 5~7 parts it is poly-
Second, 2~4 parts of zinc acetates, 3~5 parts of antimony oxides, 1~3 part of zinc acetate, 2~4 portions of triphenyl phosphites, mixing time 8
~10min, mixing time are 1~2h, and heat temperature raising temperature is 160~180 DEG C, and the hybrid reaction time is 4~6h, is continued
Heat temperature raising temperature is 240~280 DEG C, and Temperature fall temperature is 100~120 DEG C.
Step(4)Described meter in parts by weight, 25~35 parts of self-control copolymers, 10~12 parts of modified self-controls are weighed respectively
Ludox, 8~10 parts of deionized waters, 4~6 parts of polyacrylate dispersions, 3~5 parts of potassium peroxydisulfates and 2~4 parts of itaconic acids, stirring
Temperature is 55~75 DEG C, and mixing time be 16~20min, and it is 85~95 DEG C to continue whipping temp, continue mixing time for 1~
3h, soak time are 16~20min, and drying temperature is 65~75 DEG C, and drying time is 12~16min.
Compared with other method, advantageous effects are the present invention:
(1)The present invention forms self-control copolymer using polyester and polyethers copolyreaction, because its hydrophilic antistatic property derives from
Polyether segment, washability is from polyester segment and the film forming procedure of whole polymer, and wherein the strong degree of film is with polymerizeing
Thing molecular weight is relevant, and molecular weight is bigger, film more strong and washability better, polyester segment and anti-static fabric molecular structure phase
Together, eutectic is formed after heat treatment, promotes its washability to improve, so as to improve the washability of antistatic additive, and due to polyester chain
The more, washability better, and can infiltrate into inside anti-static fabric fiber molecule section, so as to improve the washability of antistatic additive,
After polyacrylate dispersion moisture evaporation, one layer of insoluble epithelium is formed in anti-static fabric fiber surface, then
Initiator and cross-linking monomer are added, strengthens the fastness of epithelium, increases the degree of cross linking after film forming, improves the resistance to of antistatic additive again
Washing property;
(2)The present invention carries out hydrophobically modified by adding Ludox, and with hydrophobic substance to Ludox, makes methyl trimethoxy epoxide silicon
Intermolecular dehydration occurs for silanol caused by alkane hydrolysis and a part of hydroxyl of silica particle surface in Ludox, then adds
Enter MethylethoxylsiliconFluid Fluid, caused silanol continues that intermolecular take off occurs with the remaining hydroxyl of silica particle surface after hydrolysis
Water is reacted, and modified Ludox is effectively filled in inside antistatic base substrate, makes it difficult for drop-off with anti-static fabric, on the contrary
More firmly, so as to improve the washability of antistatic additive, finally it is immersed in and self-control solution is mixed by sericin powder and citric acid
In, because sericin powder is anchored on anti-static fabric fiber by ester bond, washing repeatedly makes its difficult for drop-off, in addition citric acid
With the reaction of serine side base in hydroxyl in anti-static fabric and sericin powder, sericin powder is anchored at by anti-static fabric by ester bond
In, even if washing is not easy to come off repeatedly, the washability of antistatic additive is further increased, is with a wide range of applications.
Embodiment
Sericin powder and citric acid are mixed to the beaker for pouring into the deionized water with 3~5 times of sericin powder quality by same-size ratio
6~8min of middle stirring, the sodium hypophosphite of citric acid quality 40% is added after stirring, continues 20~30min of mixing, obtains
Make solution by oneself, weigh 80~90g methanol Ludox and pour into three-necked flask, three-necked flask is put into 45~65 DEG C of water-bath
16~20min is stirred, then it is 2% to add 10~12mL MTMSs and 6~8mL mass fractions into three-necked flask
MethylethoxylsiliconFluid Fluid, continue 45~60min of insulation reaction, continue into three-necked flask add 70~90g propylene glycol monomethyl ethers
Acetate mix 10~12min after, obtain react glue, will reaction glue be transferred in rotary evaporator be evaporated under reduced pressure 20~
30min, methanol is removed, obtain being modified from preparing silicon collosol, count in parts by weight, weigh 10~12 parts of terephthalic acid (TPA) diformazans respectively
Ester, 5~7 parts of polyethylene glycol mixing are placed in 8~10min of stirring in the four-hole boiling flask equipped with agitator, condenser pipe and thermometer, to
2~4 parts of zinc acetates and 3~5 parts of antimony oxides are added in four-hole boiling flask, 1~2h are mixed under the protection of nitrogen, and add
Heat is warming up to 160~180 DEG C, obtains being esterified material, continues under the protection of nitrogen, and 1~3 part of acetic acid is added into esterification material
Zinc, 2~4 parts of triphenyl phosphite 4~6h of hybrid reaction, continue to be heated to 240~280 DEG C, treat no gas effusion, natural
Be cooled to 100~120 DEG C, discharging, obtain making copolymer by oneself, count in parts by weight, weigh respectively 25~35 parts of self-control copolymers,
10~12 parts of modifications are placed in mixer from preparing silicon collosol and the mixing of 8~10 parts of deionized waters, stir 16 at 55~75 DEG C~
20min, then add 4~6 parts of polyacrylate dispersions, 3~5 parts of potassium peroxydisulfates and 2~4 parts of itaconic acids, at 85~95 DEG C after
It is continuous to mix 1~3h, room temperature is naturally cooled to, obtains antistatic base substrate, antistatic base substrate is added in self-control solution and soaked
16~20min is steeped, 12~16min of drying in 65~75 DEG C of baking oven, grinding discharging, you can high washable is made are put into after immersion
Antistatic additive.
Example 1
Sericin powder and citric acid mixed by same-size ratio and is stirred in the beaker for pouring into the deionized water with 3 times of sericin powder quality
6min, the sodium hypophosphite of citric acid quality 40% is added after stirring, continue to mix 20min, obtained making solution by oneself, weigh
80g methanol Ludox is poured into three-necked flask, and three-necked flask is put into 45 DEG C of water-bath and stirs 16min, then is burnt to three mouthfuls
10mL MTMSs and 6mL mass fractions are added in bottle as 2% MethylethoxylsiliconFluid Fluid, continues insulation reaction
45min, continue after 70g propylene glycol methyl ether acetates mixing 10min is added into three-necked flask, obtain reacting glue, will be anti-
Answer glue to be transferred in rotary evaporator and be evaporated under reduced pressure 20min, remove methanol, obtain being modified from preparing silicon collosol, count in parts by weight,
10 parts of dimethyl terephthalate (DMT)s are weighed respectively, 5 parts of polyethylene glycol mix four be placed in equipped with agitator, condenser pipe and thermometer
8min is stirred in mouth flask, 2 parts of zinc acetates and 3 parts of antimony oxides are added into four-hole boiling flask, are mixed under the protection of nitrogen
1h is stirred, and is heated to 160 DEG C, obtains being esterified material, continues under the protection of nitrogen, 1 part is added into esterification material
Zinc acetate, 2 parts of triphenyl phosphite hybrid reaction 4h, continue to be heated to 240 DEG C, treat no gas effusion, are naturally cooling to
100 DEG C, discharging, obtain making copolymer by oneself, count in parts by weight, weigh 25 parts of self-control copolymers, 10 parts of modified self-control silicon respectively
Colloidal sol and 8 parts of deionized water mixing are placed in mixer, 16min are stirred at 55 DEG C, then add 4 parts of polyacrylate dispersions, 3
Part potassium peroxydisulfate and 2 parts of itaconic acids, continue to mix 1h at 85 DEG C, naturally cool to room temperature, obtain antistatic base substrate, will
Antistatic base substrate, which is added in self-control solution, soaks 16min, is put into after immersion in 65 DEG C of baking oven and dries 12min, grinding discharging,
It can be prepared by high washable antistatic additive.
Example 2
Sericin powder and citric acid mixed by same-size ratio and is stirred in the beaker for pouring into the deionized water with 4 times of sericin powder quality
7min, the sodium hypophosphite of citric acid quality 40% is added after stirring, continue to mix 25min, obtained making solution by oneself, weigh
85g methanol Ludox is poured into three-necked flask, and three-necked flask is put into 55 DEG C of water-bath and stirs 18min, then is burnt to three mouthfuls
11mL MTMSs and 7mL mass fractions are added in bottle as 2% MethylethoxylsiliconFluid Fluid, continues insulation reaction
55min, continue after 80g propylene glycol methyl ether acetates mixing 11min is added into three-necked flask, obtain reacting glue, will be anti-
Answer glue to be transferred in rotary evaporator and be evaporated under reduced pressure 25min, remove methanol, obtain being modified from preparing silicon collosol, count in parts by weight,
11 parts of dimethyl terephthalate (DMT)s are weighed respectively, 6 parts of polyethylene glycol mix four be placed in equipped with agitator, condenser pipe and thermometer
9min is stirred in mouth flask, 3 parts of zinc acetates and 4 parts of antimony oxides are added into four-hole boiling flask, are mixed under the protection of nitrogen
1.5h is stirred, and is heated to 170 DEG C, obtains being esterified material, continues under the protection of nitrogen, 2 are added into esterification material
Part zinc acetate, 3 parts of triphenyl phosphite hybrid reaction 5h, continue to be heated to 260 DEG C, treat no gas effusion, Temperature fall
To 110 DEG C, discharging, obtain making copolymer by oneself, count in parts by weight, weigh 30 parts of self-control copolymers, 11 parts of modified self-controls respectively
Ludox and 9 parts of deionized water mixing are placed in mixer, 18min are stirred at 65 DEG C, then add 5 parts of polyacrylate breasts
Liquid, 4 parts of potassium peroxydisulfates and 3 parts of itaconic acids, continue to mix 2h at 90 DEG C, naturally cool to room temperature, obtain antistatic base
Body, antistatic base substrate is added in self-control solution and soaks 18min, is put into after immersion in 70 DEG C of baking oven and dries 14min, is ground
Discharging, you can high washable antistatic additive is made.
Example 3
Sericin powder and citric acid mixed by same-size ratio and is stirred in the beaker for pouring into the deionized water with 5 times of sericin powder quality
8min, the sodium hypophosphite of citric acid quality 40% is added after stirring, continue to mix 30min, obtained making solution by oneself, weigh
90g methanol Ludox is poured into three-necked flask, and three-necked flask is put into 65 DEG C of water-bath and stirs 20min, then is burnt to three mouthfuls
12mL MTMSs and 8mL mass fractions are added in bottle as 2% MethylethoxylsiliconFluid Fluid, continues insulation reaction
60min, continue after 90g propylene glycol methyl ether acetates mixing 12min is added into three-necked flask, obtain reacting glue, will be anti-
Answer glue to be transferred in rotary evaporator and be evaporated under reduced pressure 30min, remove methanol, obtain being modified from preparing silicon collosol, count in parts by weight,
12 parts of dimethyl terephthalate (DMT)s are weighed respectively, 7 parts of polyethylene glycol mix four be placed in equipped with agitator, condenser pipe and thermometer
8~10min is stirred in mouth flask, 4 parts of zinc acetates and 5 parts of antimony oxides are added into four-hole boiling flask, under the protection of nitrogen
2h is mixed, and is heated to 180 DEG C, obtains being esterified material, continues under the protection of nitrogen, is added into esterification material
3 parts of zinc acetates, 4 parts of triphenyl phosphite hybrid reaction 6h, continue to be heated to 280 DEG C, treat no gas effusion, Temperature fall
To 120 DEG C, discharging, obtain making copolymer by oneself, count in parts by weight, weigh 35 parts of self-control copolymers, 12 parts of modified self-controls respectively
Ludox and 10 parts of deionized water mixing are placed in mixer, 20min are stirred at 75 DEG C, then add 6 parts of polyacrylate breasts
Liquid, 5 parts of potassium peroxydisulfates and 4 parts of itaconic acids, continue to mix 3h at 95 DEG C, naturally cool to room temperature, obtain antistatic base
Body, antistatic base substrate is added in self-control solution and soaks 20min, is put into after immersion in 75 DEG C of baking oven and dries 16min, is ground
Discharging, you can high washable antistatic additive is made.
Comparative example
With the high washable antistatic additive of Guangzhou company production as a comparison case
High washable antistatic additive in high washable antistatic additive produced by the present invention and comparative example is subjected to performance detection, inspection
Survey shown under result:
1st, method of testing:
Washing fastness method of testing:Prepare the dacron of four pieces of formed objects, will be antistatic in example 1~3 and comparative example
Agent is weaved cotton cloth to terylene does antistatic treatment, is then washed in clear water after 30 times, detection hydrophily, capillary effect, surface specific resistance.
Table 1
Test event | Example 1 | Example 2 | Example 3 | Comparative example |
Hydrophily(s) | Less than 1 | Less than 1 | Less than 1 | 1 |
Capillary effect(30min)(cm) | 23 | 24 | 25 | 6 |
Surface specific resistance(Ω) | 5.2×108 | 5.1×108 | 5×108 | 5×109 |
High washable antistatic additive produced by the present invention is understood after the washing of 30 times according to data in table 1, hydrophilicity
Good with capillary effect, sheet resistance is low, antistatic effect is good, and washing fastness is high, has broad application prospects.
Claims (5)
1. a kind of preparation method of high washable antistatic additive, it is characterised in that specifically preparation process is:
(1)Sericin powder and citric acid are mixed and stirred in the beaker for pouring into the deionized water with 3~5 times of sericin powder quality, is stirred
The sodium hypophosphite of citric acid quality 40% is added after mixing, continues to mix, obtains making solution by oneself;
(2)Weigh 80~90g methanol Ludox to pour into three-necked flask, three-necked flask is put into water-bath and stirred, then to three
10~12mL MTMSs and 6~8mL MethylethoxylsiliconFluid Fluids are added in mouth flask, continues insulation reaction, is continued
After adding the mixing of 70~90g propylene glycol methyl ether acetates into three-necked flask, obtain reacting glue, reaction glue is transferred to rotation
Turn evaporator for decompression distillation, remove methanol, obtain modified from preparing silicon collosol;
(3)Count in parts by weight, weigh dimethyl terephthalate (DMT) respectively, polyethylene glycol mixing is placed in equipped with agitator, condensation
Stirred in the four-hole boiling flask of pipe and thermometer, zinc acetate and antimony oxide are added into four-hole boiling flask, under the protection of nitrogen
Mix, and heat temperature raising, obtain being esterified material, continue under the protection of nitrogen, zinc acetate, Asia are added into esterification material
Triphenyl phosphate hybrid reaction, continue heat temperature raising, treat no gas effusion, Temperature fall, discharging, obtain making copolymer by oneself;(4)
Count in parts by weight, weigh self-control copolymer respectively, be modified to mix to be placed in mixer from preparing silicon collosol and deionized water and stir,
Polyacrylate dispersion, potassium peroxydisulfate and itaconic acid are added again, continues to mix, naturally cools to room temperature, are obtained antistatic
Base substrate, antistatic base substrate is added in self-control solution and soaked, is put into baking oven and dries after immersion, grinding discharging, you can be made
High washable antistatic additive.
A kind of 2. preparation method of high washable antistatic additive according to claim 1, it is characterised in that:Step(1)Institute
The sericin powder and the same-size ratio of citric acid stated, mixing time are 6~8min, and continuation mixing time is 20~30min.
A kind of 3. preparation method of high washable antistatic additive according to claim 1, it is characterised in that:Step(2)Institute
The whipping temp stated is 45~65 DEG C, and mixing time is 16~20min, and the mass fraction of MethylethoxylsiliconFluid Fluid is 2%, reaction
Time is 45~60min, and continuation mixing time is 10~12min, and the vacuum distillation time is 20~30min.
A kind of 4. preparation method of high washable antistatic additive according to claim 1, it is characterised in that:Step(3)Institute
The meter in parts by weight stated, weigh respectively 10~12 parts of dimethyl terephthalate (DMT)s, 5~7 parts of poly- second, 2~4 parts of zinc acetates, 3~
5 parts of antimony oxides, 1~3 part of zinc acetate, 2~4 portions of triphenyl phosphites, mixing time are 8~10min, mix the time
For 1~2h, heat temperature raising temperature is 160~180 DEG C, and the hybrid reaction time be 4~6h, continue heat temperature raising temperature for 240~
280 DEG C, Temperature fall temperature is 100~120 DEG C.
A kind of 5. preparation method of high washable antistatic additive according to claim 1, it is characterised in that:Step(4)Institute
The meter in parts by weight stated, 25~35 parts of self-control copolymers, 10~12 parts of modifications are weighed respectively and are gone from preparing silicon collosol, 8~10 parts
Ionized water, 4~6 parts of polyacrylate dispersions, 3~5 parts of potassium peroxydisulfates and 2~4 parts of itaconic acids, whipping temp are 55~75 DEG C,
Mixing time is 16~20min, and it is 85~95 DEG C to continue whipping temp, and continuations mixing time is 1~3h, soak time for 16~
20min, drying temperature are 65~75 DEG C, and drying time is 12~16min.
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