CN115386058A - Preparation process of high-solid-content melamine formaldehyde resin for impregnated paper - Google Patents
Preparation process of high-solid-content melamine formaldehyde resin for impregnated paper Download PDFInfo
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- CN115386058A CN115386058A CN202211165403.2A CN202211165403A CN115386058A CN 115386058 A CN115386058 A CN 115386058A CN 202211165403 A CN202211165403 A CN 202211165403A CN 115386058 A CN115386058 A CN 115386058A
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- resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/47—Condensation polymers of aldehydes or ketones
- D21H17/49—Condensation polymers of aldehydes or ketones with compounds containing hydrogen bound to nitrogen
- D21H17/51—Triazines, e.g. melamine
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/50—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by form
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention belongs to the technical field of polymer adhesives, and relates to a preparation process of high-solid-content melamine formaldehyde resin for impregnated paper, which comprises the following steps: pumping formaldehyde which accounts for 39-41% of the total weight of the resin into a reaction kettle, adding water which accounts for 8-10% of the total weight of the resin, fully stirring, adjusting the pH to 9.0-9.5 by using a sodium hydroxide solution which accounts for 30% of the total weight of the resin, keeping the temperature to 25-30 ℃, sequentially adding melamine and diethylene glycol, stirring, heating to 90 ℃, keeping the temperature for 10min, and adding the remaining 4-6% of formaldehyde; keeping the temperature at 92-95 ℃ for reaction for 10min, adding caprolactam after the fog point of 20 ℃, slightly cooling, naturally cooling to normal temperature when the water solubility ratio is detected to be 1. The solid content of the resin is controlled by the amounts of water, diethylene glycol and caprolactam, and the storage period of the resin is prolonged, so that the wide adaptability of the resin is improved; the prepared resin has solid content of 59-62% and viscosity of 20-24s @20 ℃.
Description
Technical Field
The invention belongs to the technical field of high-molecular adhesives, relates to melamine formaldehyde resin, and particularly relates to a preparation process of high-solid-content melamine formaldehyde resin for impregnated paper.
Background
Melamine formaldehyde resins are polymers of linear networks obtained by reacting melamine with formaldehyde, also known as melamine resins (MF for english abbreviation). The preparation method is characterized in that melamine and 37 mass percent aqueous formaldehyde solution are heated to carry out addition reaction under the alkalescent condition according to the molar ratio of 1.6-2.2 to generate different numbers of N-methylol melamine derivatives, and the polycondensation reaction is further carried out along with the temperature rise to generate insoluble melamine formaldehyde resin with a stable network structure. The resin can be used for adhesives of fireproof plates, impregnating glue of decorative paper of floor furniture plates, coatings, plastic products, hardening agents and the like.
At present, the research on the melamine formaldehyde resin with high solid content is numerous, but the melamine formaldehyde resin is mostly used in other industries and cannot meet the production of impregnated paper.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to disclose a preparation process of high-solid-content melamine formaldehyde resin for impregnated paper.
Technical scheme
A preparation process of high-solid-content melamine formaldehyde resin for impregnated paper comprises the following steps:
A. pumping formaldehyde accounting for 39-41% of the total weight of the resin into a reaction kettle, adding water accounting for 8-10% of the total weight of the resin, fully stirring, adjusting the pH value to 9.0-9.5 by sodium hydroxide solution accounting for 30% of the total weight of the resin, controlling the temperature of the reaction kettle to be 25-30 ℃,
B. sequentially adding melamine accounting for 38-40% of the total weight of the resin and diglycol accounting for 5-7%, stirring, heating to 90 ℃, keeping the temperature for 10min, adding the remaining 4-6% of formaldehyde, and stirring;
C. keeping the temperature at 92-95 ℃ for reaction for 10min, starting to measure the fog point, adding caprolactam accounting for 3-5% of the total weight of the resin after the fog point reaches 20 ℃, slightly cooling, starting to cool when the water solubility ratio is detected to be 1.
In the preferred embodiment of the present invention, the concentration of formaldehyde in step A is 37%.
In the preferred embodiment of the present invention, the formaldehyde added in step A accounts for 40% of the total formaldehyde content.
In a preferred embodiment of the invention, water is added in the step A, wherein the water accounts for 9 percent of the total weight of the resin.
In a preferred embodiment of the present invention, the water used in step A is tap water, filtered water or deionized water.
In the preferred embodiment of the invention, melamine accounting for 39 percent of the total weight of the resin is added in the step B.
In a preferred embodiment of the invention, diethylene glycol is added in step B in an amount of 6% by weight based on the total weight of the resin.
In a preferred embodiment of the invention, caprolactam is added in step C in an amount of 4% by weight based on the total weight of the resin.
In the preferred embodiment of the invention, the detection is performed every 10min when the water-soluble ratio is detected in the step C.
The resin prepared by the process has the solid content of 59-62 percent and the viscosity of 20-24s @20 ℃.
Advantageous effects
The solid content of the resin is controlled by the amounts of water, diethylene glycol and caprolactam, and the storage period of the resin is prolonged, so that the wide adaptability of the resin is improved; the deionized water is adopted under the condition that the conditions allow, so that the storage period of the resin is prolonged (about 5 days in the conventional process), and the storage period is 10-30 days under the condition of normal production; the addition of the diglycol can improve the refractive index of the resin, and is beneficial to improving the glossiness of the board surface after pressing; the addition of caprolactam can improve the permeability and the fluidity of the resin, is beneficial to better permeability of impregnated paper and improves the flexibility of finished paper.
Drawings
FIG. 1 is a schematic view of a production process.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
The production process of the high-solid-content melamine formaldehyde resin for the impregnated paper comprises the following steps:
the raw material ratio is as follows: (%)
1. Preparation work
Counting the solid raw materials used which have passed the test: the method comprises the following steps of (1) checking the quantity of melamine and caprolactam, the quantity of liquid raw materials of formaldehyde (37%) and filtered water, checking whether cooling water, electricity, heating steam and the like can meet the starting production requirements, checking whether a reaction kettle is clean and free of foreign matters, and checking whether a kettle bottom valve is closed;
2. pumping primary formaldehyde required by production into a metering tank through a pipeline pump for metering, and pumping into a tested reaction kettle after metering;
3. pumping deionized water into a metering tank, and pumping into a reaction kettle after metering;
4. starting the reaction kettle for stirring, adding 30% sodium hydroxide solution after uniformly stirring, and adjusting the pH value to 9.0-9.5;
5. controlling the temperature in the kettle to be 25-30 ℃, and putting quantitative melamine and metered diglycol into the reaction kettle at one time;
6. slowly heating up to 90 ℃ in about 50 minutes (the addition reaction of formaldehyde and melamine is violent during heating up, the steam pressure and temperature change are controlled), and keeping the temperature at 90 ℃;
7. paying attention to the temperature and pH change in the kettle, and keeping the temperature at 92-95 ℃ during the heat preservation period;
8. after the heat preservation is finished for ten minutes, adding secondary formaldehyde metered by a metering tank according to the process requirement, and keeping the temperature at 92-95 ℃;
9. ten minutes later, the solution fog point in the kettle begins to be detected, when the fog point reaches 20 ℃, caprolactam prepared before is added, and the temperature in the kettle is slightly reduced to 90-92 ℃;
10. after completing the addition of the caprolactam twenty minutes, starting to detect the water solubility ratio, and immediately opening circulating water to cool and terminate the solution reaction in the kettle when the water solubility ratio reaches 1;
11. after the temperature is reduced to normal temperature, various indexes are detected, the glue can be discharged into a glue tank for standby without abnormality, and the melamine formaldehyde resin for high-solid content impregnation is obtained.
Examples
A preparation process of high-solid-content melamine formaldehyde resin for impregnated paper comprises the following steps:
A. weighing 37% formaldehyde (1 400g and 80g filtered water), adding into a three-neck flask, starting a magnetic stirrer, and adjusting pH to 9.0-9.5 with 30% sodium hydroxide; keeping the temperature at 20-30 ℃, and sequentially adding 390g of weighed melamine and 50g of diethylene glycol;
B. after the addition is finished, slowly raising the temperature, and controlling the temperature to rise to 90 ℃ within 30-40 minutes; after maintaining at 90 + -2 deg.C for ten minutes, adding a measured amount of 37% formaldehyde (2) 50g, maintaining the temperature at 92-95 deg.C, taking care that the pH is not lower than 8.8;
starting to detect the fog point after C.10min (the glue solution is dripped into a beaker filled with ice water with the temperature of zero, the glue solution becomes white and is atomized and dispersed, the water temperature in the beaker is adjusted to be 0-20 ℃ at any time along with the continuous reaction, and the dripped glue solution is ensured to be atomized and dispersed); when the cloud point is at 20 +/-1 ℃, adding 30g of weighed caprolactam; slightly cooling to 90-92 deg.C, and detecting water solubility ratio (ratio of glue solution and clear water, and keeping the mixing temperature of glue solution and clear water at 20 deg.C) after 20 min;
D. detecting every ten minutes, and when the ratio of the glue solution to the water is 1; and after the glue is detected to be qualified at normal temperature, putting the glue into a container for later use.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
1. A preparation process of high solid content melamine formaldehyde resin for impregnated paper is characterized by comprising the following steps: the method comprises the following steps:
A. pumping formaldehyde accounting for 39-41% of the total weight of the resin into a reaction kettle, adding water accounting for 8-10% of the total weight of the resin, fully stirring, adjusting the pH value to 9.0-9.5 by sodium hydroxide solution accounting for 30% of the total weight of the resin, controlling the temperature of the reaction kettle to be 25-30 ℃,
B. sequentially adding melamine accounting for 38-40% of the total weight of the resin and diethylene glycol accounting for 5% -7%, stirring, heating to 90 ℃, preserving heat for 10min, adding the remaining 4-6% of formaldehyde, and stirring;
C. keeping the temperature at 92-95 ℃ for reaction for 10min, starting to measure the fog point, adding caprolactam accounting for 3-5% of the total weight of the resin after the fog point reaches 20 ℃, slightly cooling, starting to cool when the water solubility ratio is detected to be 1.
2. The process for preparing the high-solid-content melamine formaldehyde resin for impregnated paper according to claim 1, which is characterized in that: the concentration of formaldehyde in step a was 37%.
3. The process for preparing a high solid content melamine formaldehyde resin for impregnated paper according to claim 1, wherein: the formaldehyde added in the step A accounts for 40% of the total formaldehyde.
4. The process for preparing a high solid content melamine formaldehyde resin for impregnated paper according to claim 1, wherein: in the step A, water accounting for 9 percent of the total weight of the resin is added.
5. The process for preparing the high-solid-content melamine formaldehyde resin for impregnated paper according to claim 1, which is characterized in that: the water in the step A is tap water, filtered water or deionized water.
6. The process for preparing a high solid content melamine formaldehyde resin for impregnated paper according to claim 1, wherein: in step B, 39 percent of melamine is added based on the total weight of the resin.
7. The process for preparing a high solid content melamine formaldehyde resin for impregnated paper according to claim 1, wherein: and B, adding 6 percent of diethylene glycol based on the total weight of the resin in the step B.
8. The process for preparing the high-solid-content melamine formaldehyde resin for impregnated paper according to claim 1, which is characterized in that: in step C, caprolactam accounting for 4 percent of the total weight of the resin is added.
9. The process for preparing a high solid content melamine formaldehyde resin for impregnated paper according to claim 1, wherein: and C, detecting the water-solubility ratio every 10min when detecting the water-solubility ratio in the step C.
10. A high solids melamine formaldehyde resin for impregnated paper made according to any one of claims 1 to 9 wherein: the solid content of the resin is 59-62%, and the viscosity is 20-24s @20 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211165403.2A CN115386058A (en) | 2022-09-23 | 2022-09-23 | Preparation process of high-solid-content melamine formaldehyde resin for impregnated paper |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211165403.2A CN115386058A (en) | 2022-09-23 | 2022-09-23 | Preparation process of high-solid-content melamine formaldehyde resin for impregnated paper |
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| CN115386058A true CN115386058A (en) | 2022-11-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211165403.2A Pending CN115386058A (en) | 2022-09-23 | 2022-09-23 | Preparation process of high-solid-content melamine formaldehyde resin for impregnated paper |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2202255A1 (en) * | 2008-12-18 | 2010-06-30 | Basf Se | Aqueous melamine resin mixture, method for producing same and use of same to saturate absorbent carriers and compound material produced using the melamine resin material |
| CN102492385A (en) * | 2011-11-28 | 2012-06-13 | 天津市中源装饰材料有限公司 | Melamino-formaldehyde resin adhesive and preparation method |
| CN102731963A (en) * | 2011-04-14 | 2012-10-17 | 圣象（江苏）木业研究有限公司 | Mixed type impregnating resin and its preparation method |
| CN103113542A (en) * | 2011-11-17 | 2013-05-22 | 圣象（江苏）木业研究有限公司 | High-viscosity impregnated melamine resin for producing liquid wear resistant paper and preparation method of resin |
| CN108997545A (en) * | 2018-08-29 | 2018-12-14 | 吉林森工露水河刨花板有限责任公司 | Dipping melamine resin production technology |
-
2022
- 2022-09-23 CN CN202211165403.2A patent/CN115386058A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2202255A1 (en) * | 2008-12-18 | 2010-06-30 | Basf Se | Aqueous melamine resin mixture, method for producing same and use of same to saturate absorbent carriers and compound material produced using the melamine resin material |
| CN102731963A (en) * | 2011-04-14 | 2012-10-17 | 圣象（江苏）木业研究有限公司 | Mixed type impregnating resin and its preparation method |
| CN103113542A (en) * | 2011-11-17 | 2013-05-22 | 圣象（江苏）木业研究有限公司 | High-viscosity impregnated melamine resin for producing liquid wear resistant paper and preparation method of resin |
| CN102492385A (en) * | 2011-11-28 | 2012-06-13 | 天津市中源装饰材料有限公司 | Melamino-formaldehyde resin adhesive and preparation method |
| CN108997545A (en) * | 2018-08-29 | 2018-12-14 | 吉林森工露水河刨花板有限责任公司 | Dipping melamine resin production technology |
Non-Patent Citations (4)
| Title |
|---|
| LIAN HAILAN 等: "Melamine-formadehyde resin modified with diglycol-caprolactam and its application in liquid wear-resistant technology", 《JOURNAL OF NORTHEAST FORESTRY UNIVERSITY 》, vol. 42, no. 8, pages 115 - 119 * |
| 何乃叶 等: "改性剂对低压短周期三聚氰胺甲醛树脂性能的影响", 《中国胶粘剂》, vol. 18, no. 5, pages 21 - 24 * |
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