CN100445305C - Inverse emulsion synthesis process of printing paint thickener - Google Patents

Inverse emulsion synthesis process of printing paint thickener Download PDF

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Publication number
CN100445305C
CN100445305C CNB2005100225311A CN200510022531A CN100445305C CN 100445305 C CN100445305 C CN 100445305C CN B2005100225311 A CNB2005100225311 A CN B2005100225311A CN 200510022531 A CN200510022531 A CN 200510022531A CN 100445305 C CN100445305 C CN 100445305C
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China
Prior art keywords
vinylformic acid
kerosene
step
sodium hydroxide
add
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CNB2005100225311A
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Chinese (zh)
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CN1986580A (en
Inventor
赵思远
金汉强
孙雪玲
陈永平
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南化集团研究院
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Abstract

The process of synthesizing printing paint thickener includes the first adding acrylic acid solution in certain neutralization degree into kerosene containing certain amount of activator to form reverse emulsion, adding cross-linking agent N, N' -methylene bisacrylamide and/or N-hydroxymethyl acrylamide, and adding initiator redox system at low temperature to initiate reaction. The technological process has no need of removing reaction heat and reaction period of about 3 hr, and is simple and suitable for industrial production.

Description

A kind of method of reversed-phase emulsion synthetic paint printing thickening agent

Technical field:

The invention belongs to the fine chemical technology field, relate to a kind of synthetic method of paint thickener for printing.

Background technology:

The thickening material KG-401 of pigment printing use at present is the polymkeric substance of the certain molecular weight of vinylformic acid and sodium acrylate, and solid content is about 40%, mainly replaces sodium alginate to be applied to pigment printing, especially is fit to and the dispersed dye logotype.Thickening material KG-401 forms jelly rapidly and plays thickening power in water.Shortcomings such as traditional production technique is to adopt radio polymerization, and more than 10 hours, initiated polymerization obtains this product with cobalt-60 irradiation, and this technology exists that investment is big, long reaction time, popularization difficulty are big.

Summary of the invention:

The object of the invention provides a kind of novel method of synthetic paint printing thickening agent, and the product solid content is 26%~38%, further reduces production costs.

The present invention is achieved like this:

A kind of method of reversed-phase emulsion synthetic paint printing thickening agent, form reversed-phase emulsion with joining in the kerosene that contains tensio-active agent and one or both linking agents in the sodium hydroxide and behind the vinylformic acid earlier, under low temperature, add the initiator initiated polymerization, insulation back cooling discharge obtains this product.

Be exactly synthetic specifically according to following steps:

The first step at first adds vinylformic acid in reactor, the dropping sodium aqueous solution, controlled temperature are lower than 40 ℃, dropwises to emit standbyly, and concentration sodium hydroxide is 10%~30%, and the best is 18%~26%, controls acrylic acid degree of neutralization 60%~85%

Second step added tensio-active agent, linking agent in kerosene, slowly add the solution of the first step.Tensio-active agent is a fatty acid ester, can be one or both of XU 61518.10, triolein, sorbitan oleate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitol monostearate, the best is the mixture of sorbitan oleate and polyoxyethylene sorbitan monooleate; Kerosene and acrylic acid part by weight are at 1-5: 1, be preferably 1-1.5: 1, with the amount of tensio-active agent be 8%~20% of kerosene; Linking agent is N, one or both of N '-methylene-bisacrylamide or N hydroxymethyl acrylamide; The add-on of linking agent is 0.15%~5.0% of a vinylformic acid total amount.

The 3rd step, treat the reinforced back intensification that finishes, add the initiator initiated polymerization, kick off temperature is 30 ℃~50 ℃, best kick off temperature is 35 ℃~45 ℃; Initiator is the redox system that two kinds of mixtures in ammonium persulphate, Potassium Persulphate, S-WAT, the Sodium Hydrosulphite are formed, and the best is the mixture of ammonium persulphate and Sodium Hydrosulphite; Consumption is 0.05%~2.0% of a vinylformic acid amount.

The 4th step was incubated 0.5~5 hour, and best soaking time 2~3 hours is reduced to 50 ℃ with bottom discharge.

Synthetic paint stamp thickening material novel process of the present invention owing to adopted novel process, has been taked more economical operational condition, has shortened the reaction times, has reduced running cost.

Embodiment:

Further specify the present invention below in conjunction with example.

Embodiment one:

At first add the sodium hydroxide solution that 100g vinylformic acid drips 240g18% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 120g kerosene and 10g sorbitan oleate and 8g polyoxyethylene sorbitan monooleate, 0.18gN, N '-methylene-bisacrylamide, the dropwise addition of acrylic acid neutralizer dropwises and is warming up to 35 ℃, adds ammonium persulphate and Sodium Hydrosulphite 1.5g, both weight ratios are 2: 1, cause and heat up, insulation 2h, cooling discharge.Product solid content 29%, thickening effectiveness are 15 times.

Embodiment two:

At first add the sodium hydroxide solution that 120g vinylformic acid drips 240g20% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 150g kerosene and 12g sorbitan oleate and 10g polyoxyethylene sorbitan monooleate, 1.6gN, N '-methylene-bisacrylamide, the dropwise addition of acrylic acid neutralizer dropwises and is warming up to 40 ℃, adds ammonium persulphate and Sodium Hydrosulphite 0.72g, both weight ratios are 2: 1, cause and heat up, insulation 3h, cooling discharge.Product solid content 31%, thickening effectiveness are 16 times

Embodiment three

At first add the sodium hydroxide solution that 100g vinylformic acid drips 240g20% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 120g kerosene and 10g sorbitan oleate and 9g polyoxyethylene sorbitan monooleate, 4.8gN, N '-methylene-bisacrylamide, the dropwise addition of acrylic acid neutralizer dropwises and is warming up to 45 ℃, adds ammonium persulphate and Sodium Hydrosulphite 1.2g, both weight ratios are 2: 1, initiated polymerization, insulation 2h, cooling discharge.Product solid content 30%, thickening effectiveness are 18 times

Embodiment four

At first add the sodium hydroxide solution that 100g vinylformic acid drips 200g20% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 120g kerosene and 10g sorbitan oleate and 9g polyoxyethylene sorbitan monooleate, 3.5gN-n-methylolacrylamide, the dropwise addition of acrylic acid neutralizer, dropwise and be warming up to 45 ℃, add ammonium persulphate and Sodium Hydrosulphite 1.8g, both weight ratios are 2: 1, initiated polymerization, insulation 2h, cooling discharge.Product solid content 32%, thickening effectiveness are 15 times.

Embodiment five

At first add the sodium hydroxide solution that 120g vinylformic acid drips 200g25% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 120g kerosene and 10g sorbitan oleate and 9g polyoxyethylene sorbitan monooleate, 3.5gN-n-methylolacrylamide, the dropwise addition of acrylic acid neutralizer, dropwise and be warming up to 40 ℃, add ammonium persulphate and Sodium Hydrosulphite 1.8g, both weight ratios are 2: 1, initiated polymerization, insulation 2h, cooling discharge.Product solid content 36%, thickening effectiveness are 18 times.

Embodiment six

At first add the sodium hydroxide solution that 120g vinylformic acid drips 200g25% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 120g kerosene and 10g sorbitan oleate and 9g polyoxyethylene sorbitan monooleate, 3.5gN-n-methylolacrylamide, the dropwise addition of acrylic acid neutralizer, dropwise and be warming up to 40 ℃, add ammonium persulphate and Sodium Hydrosulphite 1.8g, both weight ratios are 2: 1, initiated polymerization, insulation 2h, cooling discharge.Product solid content 36%, thickening effectiveness are 20 times.

Embodiment seven

At first add the sodium hydroxide solution that 120g vinylformic acid drips 250g20% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, and the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 120g kerosene and 10g triolein and 9g XU 61518.10,3.5gN-n-methylolacrylamide, dropwise addition of acrylic acid neutralizer, dropwise and be warming up to 40 ℃, add ammonium persulphate and Sodium Hydrosulphite 1.6g, both weight ratios are 2: 1, initiated polymerization, insulation 2h, cooling discharge.Product solid content 36%, thickening effectiveness are 12 times.

Embodiment eight

At first add the sodium hydroxide solution that 120g vinylformic acid drips 200g25% in the 1500mL four-hole boiling flask, the control neutral temperature is lower than 40 ℃, and the discharging that finishes neutralizes, this material is called the vinylformic acid neutralizer, claim 120g kerosene and 18g sorbitan oleate, 3.5gN-n-methylolacrylamide, dropwise addition of acrylic acid neutralizer, dropwise and be warming up to 40 ℃, add ammonium persulphate and Sodium Hydrosulphite 1.8g, both weight ratios are 2: 1, initiated polymerization, insulation 2h, cooling discharge.Product solid content 35%, thickening effectiveness are 15 times.

Claims (3)

1. the method for a reversed-phase emulsion synthetic paint printing thickening agent is characterized in that comprising following consecutive steps:
The first step is with in the aqueous sodium hydroxide solution and vinylformic acid, and controlled temperature is lower than 40 ℃, and neutralization finishes and emits standbyly, and the percentage concentration of sodium hydroxide is 10%~30%, controls acrylic acid degree of neutralization 60%~85%;
Second step added tensio-active agent, linking agent in kerosene, the solution that adds the first step, tensio-active agent is one or both of XU 61518.10, triolein, sorbitan oleate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitol monostearate, kerosene and acrylic acid part by weight are at (1-5): 1, and the amount of tensio-active agent is 8%~20% of a kerosene weight; Linking agent is N, one or both of N '-methylene-bisacrylamide or N hydroxymethyl acrylamide; The add-on of linking agent is 0.15%~5.0% of a vinylformic acid gross weight;
The 3rd step, treat the reinforced back intensification that finishes, add the initiator initiated polymerization, kick off temperature is 30 ℃~50 ℃, initiator is that two kinds of materials in ammonium persulphate, Potassium Persulphate, S-WAT, the Sodium Hydrosulphite mix the redox system of forming, and consumption is 0.05%%~2.0% of a vinylformic acid weight;
The 4th step was incubated 0.5~5 hour, reduced to 50 ℃ with bottom discharge.
2. method of synthetic thickening agent according to claim 1, the percentage concentration that it is characterized in that sodium hydroxide solution is 18%~26%.
3. the method for synthetic thickening agent according to claim 1 is characterized in that kick off temperature is 35 ℃~45 ℃.
CNB2005100225311A 2005-12-22 2005-12-22 Inverse emulsion synthesis process of printing paint thickener CN100445305C (en)

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Publication number Priority date Publication date Assignee Title
WO2015136438A1 (en) * 2014-03-11 2015-09-17 G.R.S. Chemical Technologies S.R.L. New polyelectrolytic polymers, process for their preparation and uses thereof

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CN101613433B (en) * 2009-07-28 2011-08-31 南京工业大学 Method for synthesizing electrolyte-resistant thickener by using inverse emulsion
CN101736608B (en) * 2009-12-15 2012-09-12 荆州市天翼精细化工开发有限公司 Pigment printing thickener and method for preparing same
CN102101909B (en) * 2009-12-18 2012-11-21 广州熵能聚合物技术有限公司 Water soluble polyurethane associative thickener, and inverse polymerization method and use thereof
CN101775099B (en) * 2010-03-10 2012-10-03 杭州传化精细化工有限公司 Paint thickener for printing and preparation method thereof
CN102153694B (en) * 2011-01-28 2013-10-30 常州大学 Inkjet printing thickener and method for preparing same
CN102720059A (en) * 2012-06-20 2012-10-10 浙江华泰丝绸有限公司 Pretreatment method for numerical printing of silk

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US4423199A (en) * 1982-09-30 1983-12-27 Rohm And Haas Company Acrylamide containing emulsion copolymers for thickening purposes
CN1152053A (en) * 1996-09-14 1997-06-18 青岛化工学院 Hyperconcentrated demulsification polymerization to produce printing thickening agent

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015136438A1 (en) * 2014-03-11 2015-09-17 G.R.S. Chemical Technologies S.R.L. New polyelectrolytic polymers, process for their preparation and uses thereof
US9771437B2 (en) 2014-03-11 2017-09-26 Italmatch Chemicals S.P.A. Polyelectrolytic polymers, process for their preparation and uses thereof
AU2015228422B2 (en) * 2014-03-11 2018-08-16 Italmatch Chemicals S.P.A. New polyelectrolytic polymers, process for their preparation and uses thereof

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