CN109942769B - A kind of processing method of stiffener - Google Patents
A kind of processing method of stiffener Download PDFInfo
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- CN109942769B CN109942769B CN201910194485.5A CN201910194485A CN109942769B CN 109942769 B CN109942769 B CN 109942769B CN 201910194485 A CN201910194485 A CN 201910194485A CN 109942769 B CN109942769 B CN 109942769B
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- China
- Prior art keywords
- formaldehyde
- stiffening agent
- reaction
- melamine
- methanol
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- 239000003351 stiffener Substances 0.000 title claims abstract description 35
- 238000003672 processing method Methods 0.000 title claims abstract description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 134
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 13
- 238000006266 etherification reaction Methods 0.000 claims abstract description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 7
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 229930040373 Paraformaldehyde Natural products 0.000 claims abstract description 5
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims abstract description 5
- 229920002866 paraformaldehyde Polymers 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000010409 thin film Substances 0.000 claims abstract description 5
- 239000008098 formaldehyde solution Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 24
- 239000007788 liquid Substances 0.000 abstract description 15
- 238000007031 hydroxymethylation reaction Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000012224 working solution Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000006276 transfer reaction Methods 0.000 description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical class O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 description 1
- HANVTCGOAROXMV-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine;urea Chemical compound O=C.NC(N)=O.NC1=NC(N)=NC(N)=N1 HANVTCGOAROXMV-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a processing method of a stiffening agent, which comprises the following steps: 1. adding a formaldehyde aqueous solution, melamine, methanol and phthalic anhydride into a reaction kettle, heating to 60 ℃ to perform a hydroxymethylation reaction for 1h, wherein the molar parts of the formaldehyde, the melamine and the methanol are 5 parts, 1 part and 4.5 parts respectively, and the mass of the phthalic anhydride accounts for 5 per thousand of the total mass; 2. continuously adding 1 part of methanol, 0.5 part of urea and 0.5 part of paraformaldehyde into the reaction kettle according to the molar parts, and heating to 80 ℃ to carry out etherification reaction for 2 hours; 3. distilling with a thin film evaporator for 1h until the solid content is 70%, discharging. The processing method of the stiffening agent is high in processing efficiency, effectively reduces the formaldehyde content in a finished product of the stiffening agent, reduces the residual formaldehyde content in the processed fabric, reduces harm to a human body, improves the stiffening effect, reduces the formaldehyde content in residual liquid after use, reduces the residual liquid treatment cost, and is more environment-friendly.
Description
Technical Field
The invention belongs to the technical field of stiffening agent processing methods, and particularly relates to a stiffening agent processing method.
Background
Stiffening agents are materials used to improve the appearance of fabrics, increase fabric elasticity and fullness, and impart stiffness. The domestic stiffening agent market mainly takes modified melamine formaldehyde resin or melamine-urea-formaldehyde resin as a main part, and the stiffening agent contains a small amount of formaldehyde due to the reasons of preparation process, raw material formula and the like, the stiffening agent is generally carried out in three reaction kettles in the processing process, the materials are mixed in a first reaction kettle, the hydroxymethylation reaction is carried out in a second reaction kettle, then the etherification reaction is carried out in a third reaction kettle, the transfer reaction kettle wastes a large amount of transfer time (three or four hours is used for transferring materials in a single reaction), incomplete reaction of formaldehyde participating in the hydroxymethylation reaction is easily caused, a large amount of formaldehyde is remained, the remained formaldehyde can generate greater harm to a human body, the purity of the stiffening agent is reduced, the use effect of the stiffening agent is influenced, and the content of the formaldehyde remained in the processed fabric is high, the stiffening agent is harmful to human bodies, and the treatment cost of residual formaldehyde in residual liquid after the stiffening agent is used is very high, so that the risk of environmental pollution is increased.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the processing method of the stiffening agent, which can improve the processing efficiency of the stiffening agent, effectively reduce the formaldehyde content in the stiffening agent, reduce the residual formaldehyde content in the processed fabric, reduce the harm to human bodies, reduce the formaldehyde content in the residual liquid after the use, reduce the residual liquid treatment cost and is more environment-friendly.
In order to solve the technical problem, the invention is solved by the following technical scheme: a processing method of a stiffening agent comprises the following steps: 1. adding a formaldehyde aqueous solution, melamine, methanol and phthalic anhydride into a reaction kettle, heating to 60 ℃ to perform a hydroxymethylation reaction for 1h, wherein the molar parts of the formaldehyde, the melamine and the methanol are respectively 5 parts, 1 part and 4.5 parts, and the mass of the phthalic anhydride accounts for 5 per thousand of the total mass of the formaldehyde, the melamine and the methanol; 2. continuously adding 1 part of methanol, 0.5 part of urea and 0.5 part of paraformaldehyde into the reaction kettle according to the molar parts, and heating to 80 ℃ to carry out etherification reaction for 2 hours; 3. distilling with a thin film evaporator for 1h until the solid content is more than or equal to 70%, discharging. The processing method of the stiffening agent has the advantages that the burdening, the hydroxymethylation reaction and the etherification reaction are all carried out in one reaction kettle during processing, so that the time for transferring a large amount of materials is reduced, meanwhile, the formaldehyde which does not participate in the hydroxymethylation reaction can directly enter the next etherification reaction, the formaldehyde content in the finished product of the stiffening agent is effectively reduced, the formaldehyde content in the residual liquid after the use is finished is reduced, the residual formaldehyde content in the processed fabric is reduced, the harm to a human body is reduced, the stiffening effect is improved, the residual liquid treatment cost is reduced, and the method is more environment-friendly.
In the above technical solution, preferably, the aqueous formaldehyde solution is a 44% aqueous formaldehyde solution.
In the above technical solution, preferably, the purity of the melamine is 99% or more.
Compared with the prior art, the invention has the following beneficial effects: the processing method of the stiffening agent has the advantages that the burdening, the hydroxymethylation reaction and the etherification reaction are all carried out in one reaction kettle during processing, so that the time for transferring a large amount of materials is reduced, meanwhile, the formaldehyde which does not participate in the hydroxymethylation reaction can directly enter the next etherification reaction, the formaldehyde content in the finished product of the stiffening agent is effectively reduced, the formaldehyde content in the residual liquid after the use is finished is reduced, the residual formaldehyde content in the processed fabric is reduced, the harm to a human body is reduced, the stiffening effect is improved, the residual liquid treatment cost is reduced, and the method is more environment-friendly.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments below: in the examples, 44% formaldehyde solution 7282g (100 mol), melamine 2522g (20 mol), methanol 2884g (90 mol), and phthalic anhydride 42g (0.284 mol) were mixed, and the mixture was heated to 60 ℃ to conduct the methylolation reaction for 1 hour; then 640.8g (20 mol) of methanol, 606g (10 mol) of urea and 300g of paraformaldehyde are added, the temperature is raised to 80 ℃ for etherification reaction for 2h, finally, a thin film evaporator is adopted for distillation for 1h until the solid content is more than or equal to 70%, and discharging is carried out.
The formaldehyde content of the stiffening agent prepared in the example was measured to obtain 0.2% formaldehyde.
The application performance of the stiffening agent prepared in the embodiment is tested, and the polyester oxford padding resin working solution (50 g/L of stiffening agent, TF-630C10 g/L of catalyst and 70% of rolling residual rate) is selected, then the polyester oxford padding resin working solution is baked at 190 ℃ for 40S, and the test is carried out after the polyester oxford padding resin working solution is dampened for 2 hours. The stiffness of the fabric is tested by a fabric stiffness tester, and the bending length of the fabric is measured to be 55.6/mm. The cloth cover formaldehyde content test standard refers to GB/T2912.2-1998 fabric formaldehyde determination part II-formaldehyde (steam absorption method) to obtain a detection result that the cloth cover formaldehyde content is 17.3 ppm. The detection concentration of the free formaldehyde content of the residual liquid is 0.1%.
Comparative example A44% formaldehyde solution 7282g (100 mol), melamine 2522g (20 mol) and methanol 2884g (90 mol) were mixed and heated to 60 ℃ for the methylolation reaction for 1 h; and (3) transferring the mixture into another reaction vessel, standing for 1h (simulating the time of a transfer reaction kettle), adding 640.8g (20 mol) of methanol, 606g (10 mol) of urea and 300g of paraformaldehyde, heating to 80 ℃ to perform etherification reaction for 2h, distilling for 1h by using a thin film evaporator until the solid content is more than or equal to 70%, and discharging.
Detecting the formaldehyde content of the stiffening agent prepared in the comparative ratio to obtain the formaldehyde content of 1.1%.
The application performance of the stiffening agent prepared in proportion is tested, and the polyester oxford fabric padding resin working solution (50 g/L of stiffening agent, TF-630C10 g/L of catalyst and 70% of rolling residual rate) is selected, then baked for 40S at 190 ℃ and tested after being remoistened for 2 h. The stiffness of the fabric is tested by a fabric stiffness tester, and the bending length of the fabric is measured to be 34.2/mm. The cloth cover formaldehyde content test standard refers to GB/T2912.2-1998 Fabric Formaldehyde determination part II, formaldehyde (steam absorption method) release, and the detection result is that the cloth cover formaldehyde is 92 ppm. The detection concentration of the free formaldehyde content of the residual liquid is 0.9 percent.
According to the detection data of the embodiment and the comparative example, the processing method of the embodiment has the advantages that the detection data of each item is obviously superior to that of the comparative example, the formaldehyde content in the finished stiffening agent is obviously reduced, the fabric is safer and healthier to use, the stiffness of the fabric is obviously improved, the cloth cover formaldehyde residue is also obviously reduced, the free formaldehyde content in the residual liquid is obviously reduced, and the residual liquid treatment cost is reduced.
The processing method of the stiffening agent has the advantages that the burdening, the hydroxymethylation reaction and the etherification reaction are all carried out in one reaction kettle during processing, so that the time for transferring a large amount of materials is reduced, meanwhile, the formaldehyde which does not participate in the hydroxymethylation reaction can directly enter the next etherification reaction, the formaldehyde content in the finished product of the stiffening agent is effectively reduced, the formaldehyde content in the residual liquid after the use is finished is reduced, the residual formaldehyde content in the processed fabric is reduced, the harm to a human body is reduced, the stiffening effect is improved, the residual liquid treatment cost is reduced, and the method is more environment-friendly.
Claims (3)
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910194485.5A CN109942769B (en) | 2019-03-14 | 2019-03-14 | A kind of processing method of stiffener |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910194485.5A CN109942769B (en) | 2019-03-14 | 2019-03-14 | A kind of processing method of stiffener |
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| Publication Number | Publication Date |
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| CN109942769A CN109942769A (en) | 2019-06-28 |
| CN109942769B true CN109942769B (en) | 2021-08-13 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0864603A2 (en) * | 1997-03-10 | 1998-09-16 | Basf Aktiengesellschaft | Aqueous binders of wood-based materials |
| WO2002040564A1 (en) * | 2000-11-14 | 2002-05-23 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Melt processable amino resin based on 1,3,5-triazines and aldehydes |
| CN103665289A (en) * | 2013-12-14 | 2014-03-26 | 山东沾化奥仕化学有限公司 | Technology for synthesizing urea modified melamine methylated resin through one-step method |
| CN105178004A (en) * | 2015-06-03 | 2015-12-23 | 东华大学 | N-methylol melamine based fabric stiffening finishing agent with low formaldehyde, preparation method and application thereof |
-
2019
- 2019-03-14 CN CN201910194485.5A patent/CN109942769B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0864603A2 (en) * | 1997-03-10 | 1998-09-16 | Basf Aktiengesellschaft | Aqueous binders of wood-based materials |
| WO2002040564A1 (en) * | 2000-11-14 | 2002-05-23 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Melt processable amino resin based on 1,3,5-triazines and aldehydes |
| CN103665289A (en) * | 2013-12-14 | 2014-03-26 | 山东沾化奥仕化学有限公司 | Technology for synthesizing urea modified melamine methylated resin through one-step method |
| CN105178004A (en) * | 2015-06-03 | 2015-12-23 | 东华大学 | N-methylol melamine based fabric stiffening finishing agent with low formaldehyde, preparation method and application thereof |
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| CN109942769A (en) | 2019-06-28 |
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Denomination of invention: A kind of processing method of stiffener Effective date of registration: 20220915 Granted publication date: 20210813 Pledgee: Industrial and Commercial Bank of China Limited Shangyu sub branch Pledgor: ZHEJIANG LIAOXIANG NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2022330002222 |
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Granted publication date: 20210813 Pledgee: Industrial and Commercial Bank of China Limited Shangyu sub branch Pledgor: ZHEJIANG LIAOXIANG NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2022330002222 |