CN112553926A - High-concentration formaldehyde-free color fixing agent and preparation process thereof - Google Patents
High-concentration formaldehyde-free color fixing agent and preparation process thereof Download PDFInfo
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- CN112553926A CN112553926A CN202011614999.0A CN202011614999A CN112553926A CN 112553926 A CN112553926 A CN 112553926A CN 202011614999 A CN202011614999 A CN 202011614999A CN 112553926 A CN112553926 A CN 112553926A
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- China
- Prior art keywords
- parts
- fixing agent
- water
- ammonium chloride
- formaldehyde
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 17
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims abstract description 16
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 15
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 11
- 239000000178 monomer Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000003929 acidic solution Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009987 spinning Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- WGESLFUSXZBFQF-UHFFFAOYSA-N n-methyl-n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCN(C)CC=C WGESLFUSXZBFQF-UHFFFAOYSA-N 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/5214—Polymers of unsaturated compounds containing no COOH groups or functional derivatives thereof
- D06P1/5242—Polymers of unsaturated N-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
- C08F226/04—Diallylamine
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of spinning, in particular to a high-concentration formaldehyde-free color fixing agent and a preparation process thereof, wherein the raw materials are easy to obtain, the preparation is simple, and meanwhile, the finished product has reliable quality and is green and environment-friendly; comprises the following components in parts by weight: 15-25 parts of isoprene, 75-85 parts of dimethyl diallyl ammonium chloride, 8-10 parts of methacrylamide, 1-7 parts of acrylamide, 3-5 parts of ethyl acetate, 1-20 parts of strong acid, 1-20 parts of ammonium chloride and the balance of water; the method comprises the following steps: step one, dissolving 1-20 parts by mass of strong acid in water to obtain an acid solution; dispersing 15-25 parts of isoprene, 75-85 parts of dimethyl diallyl ammonium chloride, 8-10 parts of methacrylamide, 1-7 parts of acrylamide and 3-5 parts of ethyl acetate in water according to parts by mass to obtain a monomer solution; and step three, heating the monomer to 70 ℃ and stirring by a magnetic stirrer.
Description
Technical Field
The invention relates to the technical field of spinning, in particular to a high-concentration formaldehyde-free color fixing agent and a preparation process thereof.
Background
The color fixing agent is one of important auxiliaries in the printing and dyeing industry, and can be used for improving the color fastness of the dye on fabrics to wet treatment. The insoluble color substance can be formed on the fabric with the dye, thereby improving the washing fastness and the perspiration fastness of the color and sometimes also improving the light fastness of the color. The existing color fixing agent generally uses a color fixing agent containing formaldehyde to improve the color fastness, but the color fixing agent containing formaldehyde is eliminated in many cases with the increasing environmental awareness of people, so that the demand of printing and dyeing manufacturers on formaldehyde-free color fixing agents is increasing day by day.
Disclosure of Invention
In order to solve the technical problems, the invention provides the high-concentration formaldehyde-free color fixing agent and the preparation process thereof, wherein the raw materials are easy to obtain, the preparation is simple, the quality of a finished product is reliable, and the high-concentration formaldehyde-free color fixing agent is green and environment-friendly.
The invention relates to a high-concentration formaldehyde-free color fixing agent which comprises the following components in parts by weight: 15-25 parts of isoprene, 75-85 parts of dimethyl diallyl ammonium chloride, 8-10 parts of methacrylamide, 1-7 parts of acrylamide, 3-5 parts of ethyl acetate, 1-20 parts of strong acid, 1-20 parts of ammonium chloride and the balance of water.
The invention relates to a high-concentration formaldehyde-free color fixing agent, which comprises the following components in parts by mass: 20 parts of isoprene, 80 parts of dimethyl diallyl ammonium chloride, 9 parts of methacrylamide, 6 parts of acrylamide, 4 parts of ethyl acetate, 1-4 parts of strong acid, 1-20 parts of ammonium chloride and the balance of water.
According to the high-concentration formaldehyde-free color fixing agent disclosed by the invention, hydrochloric acid is preferably selected as the strong acid, the concentration of the hydrochloric acid is 37%, the mass part of the hydrochloric acid is 2 parts, and the mass part of water is 160-200 parts.
According to the high-concentration formaldehyde-free color fixing agent disclosed by the invention, sulfuric acid is preferably used as the strong acid, the concentration of the sulfuric acid is 98%, the mass part of the sulfuric acid is 3 parts, and the mass part of water is 160-200 parts.
The high-concentration formaldehyde-free color fixing agent provided by the invention comprises 180 parts of water by mass.
The invention relates to a preparation process of a high-concentration formaldehyde-free color fixing agent, which comprises the following steps:
step one, dissolving 1-20 parts by mass of strong acid in water to obtain an acid solution;
dispersing 15-25 parts of isoprene, 75-85 parts of dimethyl diallyl ammonium chloride, 8-10 parts of methacrylamide, 1-7 parts of acrylamide and 3-5 parts of ethyl acetate in water according to parts by mass to obtain a monomer solution;
step three, heating the monomer to 70 ℃, and stirring by using a magnetic stirrer, wherein the heating rate in the process of heating to 70 ℃ is 1.0 ℃ per minute;
dripping the acidic solution into the monomer solution, keeping the stirring state, cooling and discharging to obtain a formaldehyde-free fixing agent solution;
and step five, drying the formaldehyde-free fixing agent solution to obtain the high-concentration formaldehyde-free fixing agent.
The invention has the beneficial effects that: the product is free of formaldehyde, is beneficial to environmental protection, is easy to obtain raw materials, is simple to prepare, and is green and environment-friendly, and the quality of a finished product is reliable.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The invention relates to a preparation process of a high-concentration formaldehyde-free color fixing agent, which comprises the following steps:
dissolving strong acid in water according to parts by mass to obtain an acid solution;
dispersing isoprene, dimethyl diallyl ammonium chloride, methacrylamide, acrylamide and ethyl acetate in water according to the mass parts to obtain a monomer solution;
step three, heating the monomer to 70 ℃, and stirring by using a magnetic stirrer, wherein the heating rate in the process of heating to 70 ℃ is 1.0 ℃ per minute;
dripping the acidic solution into the monomer solution, keeping the stirring state, cooling and discharging to obtain a formaldehyde-free fixing agent solution;
and step five, drying the formaldehyde-free fixing agent solution to obtain the high-concentration formaldehyde-free fixing agent.
Experimental group
Comprises the following components in parts by mass: 20 parts of isoprene, 80 parts of dimethyl diallyl ammonium chloride, 9 parts of methacrylamide, 6 parts of acrylamide, 4 parts of ethyl acetate, 3 parts of 98% sulfuric acid, 10 parts of ammonium chloride and the balance of water.
Comparative example 1
100 parts of dimethyl diallyl ammonium chloride, 15 parts of N-methyl diallyl amine, 6 parts of acrylic acid, 2 parts of persulfate, 1 part of bisulfite, 10 parts of ammonium acetate and the balance of water.
Comparative example 2
10 parts of isoprene, 70 parts of dimethyl diallyl ammonium chloride, 6 parts of methacrylamide, 3 parts of acrylamide, 1 part of ethyl acetate, 3 parts of 98% sulfuric acid, 7 parts of ammonium chloride and the balance of water.
Comparative example 3
14 parts of isoprene, 74 parts of dimethyl diallyl ammonium chloride, 7 parts of methacrylamide, 4 parts of acrylamide, 2 parts of ethyl acetate, 3 parts of 98% sulfuric acid, 8 parts of ammonium chloride and the balance of water.
Comparative example 4
16 parts of isoprene, 76 parts of dimethyl diallyl ammonium chloride, 8 parts of methacrylamide, 5 parts of acrylamide, 3 parts of ethyl acetate, 3 parts of 98% sulfuric acid, 9 parts of ammonium chloride and the balance of water.
Comparative example 5
24 parts of isoprene, 84 parts of dimethyl diallyl ammonium chloride, 10 parts of methacrylamide, 7 parts of acrylamide, 5 parts of ethyl acetate, 3 parts of 98% sulfuric acid, 11 parts of ammonium chloride and the balance of water.
Comparative example 6
26 parts of isoprene, 86 parts of dimethyl diallyl ammonium chloride, 11 parts of methacrylamide, 8 parts of acrylamide, 6 parts of ethyl acetate, 3 parts of 98% sulfuric acid, 12 parts of ammonium chloride and the balance of water.
The testing procedure is as per GB/T3920-2008 textile color fastness test: friction fastness was measured by the method of Friction fastness.
| Experimental group | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Fastness to boiling water | 4.4 | 4 | 4 | 4.3 | 4.4 | 4.3 | 4.2 |
| Fastness to dry rubbing | 4.5 | 3.2 | 3.6 | 4 | 4.3 | 4.2 | 4 |
| Fastness to wet rubbing | 3.6 | 2.5 | 2.8 | 3.1 | 3.4 | 3.3 | 3 |
| Color change soaping fastness | 4.2 | 3.3 | 3.5 | 3.8 | 4 | 3.8 | 3.6 |
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The high-concentration formaldehyde-free color fixing agent is characterized by comprising the following components in parts by weight: 15-25 parts of isoprene, 75-85 parts of dimethyl diallyl ammonium chloride, 8-10 parts of methacrylamide, 1-7 parts of acrylamide, 3-5 parts of ethyl acetate, 1-20 parts of strong acid, 1-20 parts of ammonium chloride and the balance of water.
2. The high-consistency formaldehyde-free fixing agent as claimed in claim 1, which comprises the following components in parts by mass: 20 parts of isoprene, 80 parts of dimethyl diallyl ammonium chloride, 9 parts of methacrylamide, 6 parts of acrylamide, 4 parts of ethyl acetate, 1-4 parts of strong acid, 1-20 parts of ammonium chloride and the balance of water.
3. The high-concentration formaldehyde-free color fixing agent as claimed in any one of claims 1 or 2, wherein the strong acid is preferably hydrochloric acid, the concentration of the hydrochloric acid is 37%, the mass part of the hydrochloric acid is 2 parts, and the mass part of the water is 160-200 parts.
4. The high-concentration formaldehyde-free color fixing agent as claimed in any one of claims 1 or 2, wherein the strong acid is preferably sulfuric acid, the concentration of the sulfuric acid is 98%, the mass part of the sulfuric acid is 3 parts, and the mass part of the water is 160-200 parts.
5. The high-consistency formaldehyde-free fixing agent as claimed in any one of claims 1 to 4, wherein the water is present in an amount of 180 parts by weight.
6. A preparation process of a high-concentration formaldehyde-free color fixing agent is characterized by comprising the following steps:
step one, dissolving 1-20 parts by mass of strong acid in water to obtain an acid solution;
dispersing 15-25 parts of isoprene, 75-85 parts of dimethyl diallyl ammonium chloride, 8-10 parts of methacrylamide, 1-7 parts of acrylamide and 3-5 parts of ethyl acetate in water according to parts by mass to obtain a monomer solution;
step three, heating the monomer to 70 ℃, and stirring by using a magnetic stirrer, wherein the heating rate in the process of heating to 70 ℃ is 1.0 ℃ per minute;
dripping the acidic solution into the monomer solution, keeping the stirring state, cooling and discharging to obtain a formaldehyde-free fixing agent solution;
and step five, drying the formaldehyde-free fixing agent solution to obtain the high-concentration formaldehyde-free fixing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011614999.0A CN112553926A (en) | 2020-12-30 | 2020-12-30 | High-concentration formaldehyde-free color fixing agent and preparation process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011614999.0A CN112553926A (en) | 2020-12-30 | 2020-12-30 | High-concentration formaldehyde-free color fixing agent and preparation process thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112553926A true CN112553926A (en) | 2021-03-26 |
Family
ID=75034776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011614999.0A Pending CN112553926A (en) | 2020-12-30 | 2020-12-30 | High-concentration formaldehyde-free color fixing agent and preparation process thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112553926A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3491064A (en) * | 1965-06-26 | 1970-01-20 | Pfersee Chem Fab | Process for producing water-soluble nitrogen-containing products by reacting a compound containing a group with formaldehyde and free amines |
| CN104420374A (en) * | 2013-09-06 | 2015-03-18 | 无锡荡口通和纺织机械厂 | Polycationic formaldehyde-free color fixing agent and preparation method thereof |
| CN104452366A (en) * | 2014-11-17 | 2015-03-25 | 太仓运通生物化工有限公司 | Formaldehyde-free color-fixing agent and preparation method of color-fixing agent |
-
2020
- 2020-12-30 CN CN202011614999.0A patent/CN112553926A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3491064A (en) * | 1965-06-26 | 1970-01-20 | Pfersee Chem Fab | Process for producing water-soluble nitrogen-containing products by reacting a compound containing a group with formaldehyde and free amines |
| CN104420374A (en) * | 2013-09-06 | 2015-03-18 | 无锡荡口通和纺织机械厂 | Polycationic formaldehyde-free color fixing agent and preparation method thereof |
| CN104452366A (en) * | 2014-11-17 | 2015-03-25 | 太仓运通生物化工有限公司 | Formaldehyde-free color-fixing agent and preparation method of color-fixing agent |
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Application publication date: 20210326 |
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