CN104387508A - Method for preparing paste resin with medium viscosity - Google Patents

Method for preparing paste resin with medium viscosity Download PDF

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Publication number
CN104387508A
CN104387508A CN201410775089.9A CN201410775089A CN104387508A CN 104387508 A CN104387508 A CN 104387508A CN 201410775089 A CN201410775089 A CN 201410775089A CN 104387508 A CN104387508 A CN 104387508A
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CN
China
Prior art keywords
latex
paste resin
vinyl chloride
chloride monomer
vitriol
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Pending
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CN201410775089.9A
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Chinese (zh)
Inventor
魏永涛
崔玉霞
田爱娟
李永胜
李益成
张东洲
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Tianjin Botian Chemical Co Ltd
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Tianjin Botian Chemical Co Ltd
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Priority to CN201410775089.9A priority Critical patent/CN104387508A/en
Publication of CN104387508A publication Critical patent/CN104387508A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for preparing paste resin with medium viscosity. The method comprises the following steps: producing the paste resin by using an emulsion polymerization method; adding a monomer and aids into a polymerizing kettle according to a formula proportion; performing vacuumizing and deoxidation, raising the temperature to 50-63 DEG C under a stirring state, performing polymerization reaction at the temperature of 50-63 DEG C, starting to reduce the pressure of 0.83MPa, and ending the reaction when the pressure is reduced to 0.4MPa. The method is characterized in that 1, the tensile strength of leather working gloves produced by using the paste resin with the medium viscosity is higher than that of common leather working gloves; 2, the glossiness of the leather working gloves produced by using the paste resin with the medium viscosity is higher than that of the common leather working gloves; 3, compared with other processes, a process of producing the leather working gloves produced by using the paste resin with the medium viscosity has the advantages of moderate viscosity and simplicity in de-foaming.

Description

A kind of method preparing middle viscosity paste resin
Technical field
The invention belongs to macromolecule chemical industry technical field, specifically a kind of production method adopting viscosity paste resin in emulsion method preparation.
Background technology
China is the production base of world's safety and industrial gloves, the sector is larger to the consumption sticking with paste resin, and only have the P737 of Sweden to be used alone at present, but price is higher, domestic rouge and powder can Some substitute P737, but there is the lacklustre phenomenon of gloves, therefore most producer adopts the paste resin of more than 3 kinds to carry out used in combinationly reaching requirement.Annual the sector should more than 100,000 tons to the consumption of resin, and the imitative rubber safety and industrial gloves consumption of non-liner is more than 20,000 tons, and to require to stick with paste resin viscosity high and be easy to deaeration for imitative rubber safety and industrial gloves at present, and goods are glossy.The sector has new processing producer to go into operation every year, and the demand of imitative rubber safety and industrial gloves is in the trend of rising.
Summary of the invention
Object of the present invention provides a kind of new emulsion method polymerization process, and the Particle size requirements of obtained paste resin, at 0.10 μm ~ 1.50 μm, prepares the paste resin of medium viscosity on this basis.
The object of the present invention is achieved like this:
A kind of method preparing middle viscosity paste resin, it is characterized in that adopting emulsion polymerization to produce, by formula rate, monomer and auxiliary agent are added polymeric kettle, through vacuumizing, deoxidation, under whipped state, be warming up to 50 ~ 63 DEG C, carry out polyreaction at this temperature, 0.83MPa pressure starts to decline, when pressure drops to 0.4MPa, reaction terminates, and detailed process is as follows:
(1) in proportion deionized water is added in polymeric kettle, under the state stirred, add the vitriol of saturated alcohol, sulphite, ph conditioning agent;
(2) then polymeric kettle vacuumize, deoxidation, add vinyl chloride monomer, by polymerization kettle temperature raising to 50 ~ 63 DEG C, add the vitriol of saturated alcohol in the course of the polymerization process continuously;
(3) joined continuously in polymeric kettle by persulfate solution good for water dissolution, keep whipped state, carry out polyreaction, control reaction at 50 ~ 63 DEG C, when 0.83MPa pressure starts to decline, when pressure drops to 0.4MPa, reaction terminates;
(4), after reaction terminates, first unreacted vinyl chloride monomer is recycled to gas holder, latex is delivered to latex storage tank;
(5) vinyl chloride monomer in air-extraction removal latex is adopted, the latex extracted out from latex storage tank by transferpump, after steam direct heating, enter stripping tower, in latex, residual monomer and a small amount of moisture content are by vacuumizing removing in tower, be recycled to gas holder by the vinylchlorid that stripping goes out, with transferpump, the latex after gas delivered to drying section by strainer;
It is (6) dry,
Stripped latex adopts spray-drying process to carry out drying treatment, requires water content≤0.4%;
(7) particle diameter of dried material is at 0.10 ~ 1.50 μm;
(8) then weigh, packaging;
Above-described vinyl chloride monomer: deionized water: persulphate: sulphite: the vitriol of saturated alcohol: the ratio of ph conditioning agent is 100:100:0.1-1:0.1-1:0.1-1:0.1-0.5.
Above-described persulphate is Potassium Persulphate; Described sulphite is sodium bisulfite; The vitriol of described saturated alcohol is sodium lauryl sulfate; Described ph conditioning agent is bicarbonate of ammonia.
Feature of the present invention is:
1. the safety and industrial gloves tensile strength adopting the safety and industrial gloves of this kind of medium viscosity paste production of resins more common is good.
2. the safety and industrial gloves glossiness using the safety and industrial gloves of this kind of medium viscosity paste production of resins more common is high.
3. be modest viscosity in the process using this kind of medium viscosity to stick with paste production of resins safety and industrial gloves compared with the advantage of other technique and be easy to deaeration.
Embodiment
Concrete enforcement 1
(1) vinyl chloride monomer, the deionized water of 12Kg, the Potassium Persulphate of 10g, the sodium bisulfite of 10g, the sodium lauryl sulfate of 160g, the bicarbonate of ammonia of 5g of 12Kg is added by above-mentioned formula.
(2) then polymeric kettle vacuumize, deoxidation, add vinyl chloride monomer by formula, by polymerization kettle temperature raising to 50 ~ 63 DEG C, add sodium lauryl sulfate continuously in the course of the polymerization process;
(3) joined continuously in polymeric kettle by potassium persulfate solution good for water dissolution, keep whipped state, carry out polyreaction, control reaction at 58.0 DEG C, when 0.89MPa pressure starts to decline, when pressure drops to 0.45MPa, reaction terminates;
(4), after reaction terminates, first unreacted vinyl chloride monomer is recycled to gas holder, latex is delivered to latex storage tank;
(5) vinyl chloride monomer in vaporizing extract process removal latex is adopted: the latex extracted out from latex storage tank by transferpump, after steam direct heating, enter stripping tower, in latex, residual monomer and a small amount of moisture content are by vacuumizing removing in tower, be recycled to gas holder by the vinylchlorid that stripping goes out, with transferpump, the latex after gas delivered to drying section by strainer;
(6) dry
Stripped latex adopts spray-drying process to carry out drying treatment, requires water content≤0.4%;
(7) particle diameter of dried material is at 0.10 ~ 1.50 μm;
(8) then weigh, packaging.
(9) material test data is mean polymerisation degree: 1050; Median size: 0.87 μm; Stick with paste resin viscosity: 10000cp.
Concrete enforcement 2
(1) vinyl chloride monomer, the deionized water of 13Kg, the Potassium Persulphate of 10g, the sodium bisulfite of 10g, the sodium lauryl sulfate of 160g, the bicarbonate of ammonia of 5g of 13Kg is added by above-mentioned formula.
(2) then polymeric kettle vacuumize, deoxidation, add vinyl chloride monomer by formula, by polymerization kettle temperature raising to 50 ~ 63 DEG C, add sodium lauryl sulfate continuously in the course of the polymerization process;
(3) joined continuously in polymeric kettle by potassium persulfate solution good for water dissolution, keep whipped state, carry out polyreaction, control reaction at 60.0 DEG C, when 1.0MPa pressure starts to decline, when pressure drops to 0.5MPa, reaction terminates;
(4), after reaction terminates, first unreacted vinyl chloride monomer is recycled to gas holder, latex is delivered to latex storage tank;
(5) vinyl chloride monomer in vaporizing extract process removal latex is adopted: the latex extracted out from latex storage tank by transferpump, after steam direct heating, enter stripping tower, in latex, residual monomer and a small amount of moisture content are by vacuumizing removing in tower, be recycled to gas holder by the vinylchlorid that stripping goes out, with transferpump, the latex after gas delivered to drying section by strainer;
(6) dry
Stripped latex adopts spray-drying process to carry out drying treatment, requires water content≤0.4%;
(7) particle diameter of dried material is at 0.10 ~ 1.50 μm;
(8) then weigh, packaging.
(9) material test data is mean polymerisation degree: 900; Median size: 0.90 μm; Stick with paste resin viscosity: 8000cp.
Concrete enforcement 3
(1) vinyl chloride monomer, the deionized water of 12Kg, the Potassium Persulphate of 10g, the sodium bisulfite of 10g, the sodium lauryl sulfate of 160g, the bicarbonate of ammonia of 5g of 12Kg is added by above-mentioned formula.
(2) then polymeric kettle vacuumize, deoxidation, add vinyl chloride monomer by formula, by polymerization kettle temperature raising to 50 ~ 63 DEG C, add sodium lauryl sulfate continuously in the course of the polymerization process;
(3) joined continuously in polymeric kettle by potassium persulfate solution good for water dissolution, keep whipped state, carry out polyreaction, control reaction at 50.5 DEG C, when 0.80MPa pressure starts to decline, when pressure drops to 0.40MPa, reaction terminates;
(4), after reaction terminates, first unreacted vinyl chloride monomer is recycled to gas holder, latex is delivered to latex storage tank;
(5) vinyl chloride monomer in vaporizing extract process removal latex is adopted: the latex extracted out from latex storage tank by transferpump, after steam direct heating, enter stripping tower, in latex, residual monomer and a small amount of moisture content are by vacuumizing removing in tower, be recycled to gas holder by the vinylchlorid that stripping goes out, with transferpump, the latex after gas delivered to drying section by strainer;
(6) dry
Stripped latex adopts spray-drying process to carry out drying treatment, requires water content≤0.4%;
(7) particle diameter of dried material is at 0.10 ~ 1.50 μm;
(8) then weigh, packaging.
(9) material test data is mean polymerisation degree: 1250; Median size: 0.95 μm; Stick with paste resin viscosity: 9000cp.

Claims (2)

1. prepare the method that middle viscosity sticks with paste resin for one kind, it is characterized in that adopting emulsion polymerization to produce, by formula rate, monomer and auxiliary agent are added polymeric kettle, through vacuumizing, deoxidation, under whipped state, be warming up to 50 ~ 63 DEG C, carry out polyreaction at this temperature, 0.83MPa pressure starts to decline, when pressure drops to 0.4MPa, reaction terminates, and detailed process is as follows:
(1) in proportion deionized water is added in polymeric kettle, under the state stirred, add the vitriol of saturated alcohol, sulphite, ph conditioning agent;
(2) then polymeric kettle vacuumize, deoxidation, add vinyl chloride monomer, by polymerization kettle temperature raising to 50 ~ 63 DEG C, add the vitriol of saturated alcohol in the course of the polymerization process continuously;
(3) joined continuously in polymeric kettle by persulfate solution good for water dissolution, keep whipped state, carry out polyreaction, control reaction at 50 ~ 63 DEG C, when 0.83MPa pressure starts to decline, when pressure drops to 0.4MPa, reaction terminates;
(4), after reaction terminates, first unreacted vinyl chloride monomer is recycled to gas holder, latex is delivered to latex storage tank;
(5) vinyl chloride monomer in air-extraction removal latex is adopted, the latex extracted out from latex storage tank by transferpump, after steam direct heating, enter stripping tower, in latex, residual monomer and a small amount of moisture content are by vacuumizing removing in tower, be recycled to gas holder by the vinylchlorid that stripping goes out, with transferpump, the latex after gas delivered to drying section by strainer;
It is (6) dry,
Stripped latex adopts spray-drying process to carry out drying treatment, requires water content≤0.4%;
(7) particle diameter of dried material is at 0.10 ~ 1.50 μm;
(8) then weigh, packaging;
Above-described vinyl chloride monomer: deionized water: persulphate: sulphite: the vitriol of saturated alcohol: the ratio of ph conditioning agent is 100:100:0.1-1:0.1-1:0.1-1:0.1-0.5.
2. in preparation according to claim 1, viscosity sticks with paste the method for resin, it is characterized in that described persulphate is Potassium Persulphate; Described sulphite is sodium bisulfite; The vitriol of described saturated alcohol is sodium lauryl sulfate; Described ph conditioning agent is bicarbonate of ammonia.
CN201410775089.9A 2014-12-15 2014-12-15 Method for preparing paste resin with medium viscosity Pending CN104387508A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106883330A (en) * 2015-12-16 2017-06-23 天津渤天化工有限责任公司 A kind of high viscosity pastes the preparation method of resin
CN106883329A (en) * 2015-12-16 2017-06-23 天津渤天化工有限责任公司 A kind of high viscosity pastes resin

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1594379A (en) * 2004-06-25 2005-03-16 杭州电化集团有限公司 Process for polymerization preparation of vinyl chloride/isobutyl vinyl ether copolyresin latex
CN1618824A (en) * 2004-01-16 2005-05-25 清华大学 Crosslinked core-shell structure nano-polymer microsphere and its preparation method
CN101205270A (en) * 2007-11-22 2008-06-25 上海氯碱化工股份有限公司 Production method of PVC paste resin for glove material
CN101591501A (en) * 2008-05-27 2009-12-02 北京高盟燕山科技有限公司 Be used for high dilution ratio aqueous coating agent of PVC powder-free gloves and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1618824A (en) * 2004-01-16 2005-05-25 清华大学 Crosslinked core-shell structure nano-polymer microsphere and its preparation method
CN1594379A (en) * 2004-06-25 2005-03-16 杭州电化集团有限公司 Process for polymerization preparation of vinyl chloride/isobutyl vinyl ether copolyresin latex
CN101205270A (en) * 2007-11-22 2008-06-25 上海氯碱化工股份有限公司 Production method of PVC paste resin for glove material
CN101591501A (en) * 2008-05-27 2009-12-02 北京高盟燕山科技有限公司 Be used for high dilution ratio aqueous coating agent of PVC powder-free gloves and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106883330A (en) * 2015-12-16 2017-06-23 天津渤天化工有限责任公司 A kind of high viscosity pastes the preparation method of resin
CN106883329A (en) * 2015-12-16 2017-06-23 天津渤天化工有限责任公司 A kind of high viscosity pastes resin

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