CN1932140A - Method for producing formeldehyde-free colour fixing agent - Google Patents
Method for producing formeldehyde-free colour fixing agent Download PDFInfo
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- CN1932140A CN1932140A CN 200610096042 CN200610096042A CN1932140A CN 1932140 A CN1932140 A CN 1932140A CN 200610096042 CN200610096042 CN 200610096042 CN 200610096042 A CN200610096042 A CN 200610096042A CN 1932140 A CN1932140 A CN 1932140A
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Abstract
The present invention relates to a preparation method of formaldehyde-free dye-fixing agent. Said method includes the following steps: (1), adding (by weight portion) 40-50 portions of ethyl acrylate, 1-2 portions of acrylic acid and 60-65 portions of sodium metabisulfite into a reaction still, stirring and uniformly mixing them, heating to 65 plus or minus 2 deg.C, heat-insulating and making reaction for 2 hr plus or minus 0.5 hr; (2), drop-adding 80-85 portions of di-ethylene triamine and controlling temperature below 70 deg.C; (3), adding proper quantity of water, after 10 min, drop-adding 70-75 portions of epichlorohydrin and controlling temperature below 70 deg.C so as to produce transparent or light yellow color, cooling; and (4), cooling to room temperature, adding concentrated hydrochloric acid to regulate pH value and make it be 6-7, regulating solid content so as to obtain the invented finished product.
Description
Technical field
The present invention relates to a kind of preparation method of environmentally friendly waterproof casein glue for sticking label onto bottle.
Background technology
Current textile dyeing is based on reactive dyeing, but because of containing hydrophilic radical in such dyestuff, and the dye particle size can have influence on the soaping fastness of dyeing.Cause wet colour fastness defective.Must use color-fixing agent to come fixation.In the past, the color-fixing agent of employing mostly was the color-fixing agent that contains formaldehyde.Restriction along with some national PARA FORMALDEHYDE PRILLS(91,95) content, make the formaldehyde color-fixing agent be eliminated, in recent years, formaldehyde-free color fixing agent often has report in some patents, as 03114001.7 aldehyde-free colour stabilizer that discloses the preparation of a kind of diethylenetriamine and epoxychloropropane, yet because of its prescription is single, effect is undesirable.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency, the preparation method of the formaldehyde-free color fixing agent of the good and environmental protection of a kind of colour fixation is provided.
The object of the present invention is achieved like this: a kind of preparation method of formaldehyde-free color fixing agent is characterized in that: this method comprises following processing step:
1) with ethyl acrylate 40-50 weight portion, acrylic acid 1-2 weight portion and sodium pyrosulfite 60-65 weight portion stir behind the adding reactor, fully mix, and are warmed up to 65 ± 2 ℃, insulation reaction 2 hours ± 0.5 hour;
2) drip diethylenetriamine 80-85 weight portion, the control temperature is below 70 ℃;
3) add suitable quantity of water, after 10 minutes, drip epoxychloropropane 70-75 weight portion again, the control temperature is below 70 ℃, occurs transparently or faint yellow, lowers the temperature;
When 4) reducing to room temperature, add concentrated hydrochloric acid and regulate pH value 6-7, behind the adjusting solid content, discharging gets finished product.
The solid content of the color-fixing agent of preparation is 20-40%.Adopt the color-fixing agent of method for preparing, can obtain high-quality colour fixation.The color-fixing agent of this invention preparation does not produce the formaldehydes material in producing and using, two keys of acrylic acid (ester) have certain cross-linking properties, and this product belongs to the cross-linking type color-fixing agent, season (uncle) ammonium salt certain electropositive is arranged.
The specific embodiment
Embodiment 1:
With ethyl acrylate 45Kg, acrylic acid 1.2KG and sodium pyrosulfite 65g add the back stirring and make its abundant mixed dissolution, are warmed up to 66 ℃, insulation reaction 2 hours in the 100Kg reactor;
It is in 60 ℃ the 500Kg reactor that still internal reaction material is transferred to preheating, drips diethylenetriamine 85KG, about 40 minutes, note variations in temperature, and can not surpass 70 ℃ in preceding 30 minutes, slowly blowing.Reacted 2.5 hours down at 65 ℃, add the 150Kg deionized water again, about 10 minutes, drip epoxychloropropane 75Kg again, dripped off in about 1 hour, (being controlled at below 70 ℃) occurs transparent or faint yellow, finishes;
Cool to below 40 ℃, the cooling room temperature, the heating concentrated hydrochloric acid, adjust pH is 6, adds surplus water, regulating solid content is 30%, filters discharging.
Embodiment 2:
With ethyl acrylate 50Kg, acrylic acid 1.0KG and sodium pyrosulfite 70g add the back stirring and make its abundant mixed dissolution, are warmed up to 65 ℃, insulation reaction 2 hours in the 100Kg reactor;
It is in 60 ℃ the 500Kg reactor that still internal reaction material is transferred to preheating, drips diethylenetriamine 82Kg, about 40 minutes, note variations in temperature, and can not surpass 70 ℃ in preceding 30 minutes, slowly blowing.Reacted 2.5 hours down at 65 ℃, add the 150Kg deionized water again, about 10 minutes, drip epoxychloropropane 70Kg again, dripped off in about 1 hour, temperature is controlled at below 70 ℃, and system occurs transparent or faint yellow, finishes;
Cool to below 40 ℃, be cooled to room temperature, adding the concentrated hydrochloric acid adjust pH is 6.5, adds surplus water, and regulating solid content is 30%, filters discharging.
Claims (1)
1, a kind of preparation method of formaldehyde-free color fixing agent is characterized in that: this method comprises following processing step:
1) with ethyl acrylate 40-50 weight portion, acrylic acid 1-2 weight portion and sodium pyrosulfite 60-65 weight portion stir behind the adding reactor, fully mix, and are warmed up to 65 ± 2 ℃, insulation reaction 2 hours ± 0.5 hour;
2) drip diethylenetriamine 80-85 weight portion, the control temperature is below 70 ℃;
3) add suitable quantity of water, after 10 minutes, drip epoxychloropropane 70-75 weight portion again, the control temperature is below 70 ℃, occurs transparently or faint yellow, lowers the temperature;
When 4) reducing to room temperature, add concentrated hydrochloric acid and regulate pH value 6-7, behind the adjusting solid content, discharging gets finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100960425A CN100395401C (en) | 2006-09-14 | 2006-09-14 | Method for producing formeldehyde-free colour fixing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100960425A CN100395401C (en) | 2006-09-14 | 2006-09-14 | Method for producing formeldehyde-free colour fixing agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1932140A true CN1932140A (en) | 2007-03-21 |
| CN100395401C CN100395401C (en) | 2008-06-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100960425A Expired - Fee Related CN100395401C (en) | 2006-09-14 | 2006-09-14 | Method for producing formeldehyde-free colour fixing agent |
Country Status (1)
| Country | Link |
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| CN (1) | CN100395401C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492138A (en) * | 2011-12-06 | 2012-06-13 | 西安工程大学 | Method for preparing polyamine-epichlorohydrin color fixing agent |
| CN103643567A (en) * | 2013-12-06 | 2014-03-19 | 成路凯尔服装（苏州）有限公司 | Synthesis method of multifunctional silk fabric fixing agent |
| CN103696297A (en) * | 2013-12-09 | 2014-04-02 | 常熟市爱博尔服饰有限公司 | Color fixing agent for wool fiber |
| CN107474178A (en) * | 2017-08-23 | 2017-12-15 | 广州中国科学院工业技术研究院 | Pigment adsorbent and preparation method thereof |
| CN107511136A (en) * | 2017-08-23 | 2017-12-26 | 广州中国科学院工业技术研究院 | The treatment fluid of pigment adsorbent and its application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100350097C (en) * | 2003-03-27 | 2007-11-21 | 三水市金盛精细化工有限公司 | Manufacturing technology of formaldehydeless colour fixing agent |
-
2006
- 2006-09-14 CN CNB2006100960425A patent/CN100395401C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492138A (en) * | 2011-12-06 | 2012-06-13 | 西安工程大学 | Method for preparing polyamine-epichlorohydrin color fixing agent |
| CN103643567A (en) * | 2013-12-06 | 2014-03-19 | 成路凯尔服装（苏州）有限公司 | Synthesis method of multifunctional silk fabric fixing agent |
| CN103696297A (en) * | 2013-12-09 | 2014-04-02 | 常熟市爱博尔服饰有限公司 | Color fixing agent for wool fiber |
| CN107474178A (en) * | 2017-08-23 | 2017-12-15 | 广州中国科学院工业技术研究院 | Pigment adsorbent and preparation method thereof |
| CN107511136A (en) * | 2017-08-23 | 2017-12-26 | 广州中国科学院工业技术研究院 | The treatment fluid of pigment adsorbent and its application |
| CN107474178B (en) * | 2017-08-23 | 2019-11-12 | 广州中国科学院工业技术研究院 | Pigment adsorbent and preparation method thereof |
| CN107511136B (en) * | 2017-08-23 | 2020-04-28 | 广州中国科学院工业技术研究院 | Pigment adsorbent treatment liquid and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100395401C (en) | 2008-06-18 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Jiangyin Ruco Technology Co., Ltd. Assignor: Hua Mingyang Contract fulfillment period: 2009.4.10 to 2014.4.10 contract change Contract record no.: 2009320000801 Denomination of invention: Method for producing formeldehyde-free colour fixing agent Granted publication date: 20080618 License type: Exclusive license Record date: 2009.5.6 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.4.10 TO 2014.4.10; CHANGE OF CONTRACT Name of requester: JIANGYIN CITY NUOKE SCIENCE CO., LTD. Effective date: 20090506 |
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