CN112940210B - Preparation method of methylated melamine formaldehyde resin - Google Patents
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- CN112940210B CN112940210B CN202110273324.2A CN202110273324A CN112940210B CN 112940210 B CN112940210 B CN 112940210B CN 202110273324 A CN202110273324 A CN 202110273324A CN 112940210 B CN112940210 B CN 112940210B
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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
- C08G12/42—Chemically modified polycondensates by etherifying
- C08G12/424—Chemically modified polycondensates by etherifying of polycondensates based on heterocyclic compounds
- C08G12/425—Chemically modified polycondensates by etherifying of polycondensates based on heterocyclic compounds based on triazines
- C08G12/427—Melamine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
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Abstract
A preparation method of methylated melamine formaldehyde resin relates to the technical field of fine chemical engineering, in particular to a preparation method of methylated melamine formaldehyde resin. The method comprises the following steps: step 1: adding formaldehyde, melamine and liquid caustic soda into a pipeline, heating to 60-70 ℃, and reacting for 10-12 min under the condition of heat preservation; the molar ratio of formaldehyde to melamine is 6.9-7.1; step 2: adjusting the pH to be 3-4, and reacting for 5-7 min in a heat preservation way; the mol ratio of melamine to methanol is 1; negative pressure distillation is carried out at 65-70 ℃; and 3, step 3: adjusting the pH = 3-4, and reacting for 4-6 min under the condition of heat preservation; the mol ratio of the melamine to the methanol is 1; then distilling to 115-120 ℃ under negative pressure, and filtering to obtain the methylated melamine formaldehyde resin. The method has the advantages of avoiding the problem of poor product quality among batches, along with easy operation, good product stability and high yield.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a preparation method of methylated melamine formaldehyde resin.
Background
The rubber adhesive is a methanol etherified melamine formaldehyde resin which is important in amino resin. At present, amino resin for coating is still in the development stage of high etherification degree methanol etherification melamine formaldehyde resin (HMMM) except butanol etherification melamine formaldehyde resin which is already mature. The invention patent with application number 2020110369056 discloses a preparation method of methylated melamine formaldehyde resin, which adopts a reaction kettle type batch method reaction preparation method, and the batch method preparation has the problem of product quality difference between each batch, and simultaneously has the disadvantages of complicated process and inconvenient operation.
Disclosure of Invention
The invention aims to provide a preparation method of methylated melamine-formaldehyde resin, which aims to solve the problem of poor product quality among batches, is easy to operate and has good product stability.
The preparation method of the methylated melamine formaldehyde resin is characterized by comprising the following steps:
step 1: quantitatively adding formaldehyde, melamine and liquid caustic soda into a pipeline, conveying at a constant speed, heating to 60-70 ℃ in the conveying process, and reacting for 10-12 min under heat preservation; in the raw materials, the molar ratio of formaldehyde to melamine is 6.9-7.1, and the PH is controlled to be 8-9;
and 2, step: after the heat preservation reaction is finished, quantitatively adding methanol into a pipeline flowing at a constant speed, controlling the temperature, then adding hydrochloric acid to adjust the pH = 3-4, preserving the heat for reaction for 5-7 min, and then quantitatively adding liquid alkali to adjust the pH = 8-9; the molar ratio of the melamine to the methanol added into the pipeline is 1; then the reaction system enters a film evaporator to carry out negative pressure distillation to 65-70 ℃;
and step 3: quantitatively adding the semi-finished product after the crude steaming and methanol into a pipeline, quantitatively adding hydrochloric acid after temperature control to adjust the pH = 3-4, carrying out heat preservation reaction for 4-6 min, and then quantitatively adding liquid caustic soda to adjust the pH = 8-9; the molar ratio of the melamine to the methanol added into the pipeline is 1 to 5; then the reaction system enters a film evaporator to carry out negative pressure distillation to 115-120 ℃, and the product of methylated melamine formaldehyde resin is obtained by filtration.
Further, the hydroxylation reaction temperature in the step 1 is 65 ℃; the molar ratio of formaldehyde to melamine in the raw materials was 7.0.
Further, in the step 1, in the heating process, the reaction system is heated by a circulating hot water heating system.
Further, in the temperature control process in the step 2, the temperature of the reaction system is controlled by a warm water heating system and a circulating water cooling system.
Further, in the step 2 and the step 3, the etherification reaction temperature is 40 ℃.
Compared with the existing preparation method of reaction kettle type batch reaction, the preparation method of methylated melamine formaldehyde resin provided by the invention has the following innovation points and beneficial effects:
1. in step 1, the reaction system is heated by water with the temperature lower than 75 ℃ so as to avoid generating a large amount of byproducts due to overhigh temperature. At this temperature, since the reaction is slow and not vigorous, the amount of by-products produced is small, and therefore a high yield of the product can be produced.
2. In the step 2, after quantitative methanol and quantitative reaction system in the step 1 are mixed, the temperature is controlled in a set range, and then hydrochloric acid is added quantitatively to adjust the pH value for etherification reaction. The etherification reaction degree under the process condition is easy to control, the product polymerization degree is effectively reduced, and the product with high yield can be produced.
3. In the step 2 and the step 3, the distilled mother liquor is sent to a rectification system to purify the methanol for reuse in the etherification process. In the step 3, the filtered liquid is a product HMMM, and the filter cake is waste sodium chloride salt and needs to be incinerated.
4. According to the invention, the tubular reaction mode of raw materials fed continuously through a pipeline is used for replacing the reaction production mode of a reaction kettle type batch method, so that the problem of quality difference of products among batches of the batch method is solved, and meanwhile, the whole process is controlled automatically, so that the operation workers are simpler.
5. The method has the advantages of small pollution, energy conservation and environmental protection, reduces the production cost, reduces the risk of potential safety hazard of the process, and has higher product yield: the content of the formaldehyde combined with the methylated melamine formaldehyde resin is 42 to 43 percent (the content index of the formaldehyde combined with the product is more than or equal to 40 percent).
The methylated melamine formaldehyde resin has high etherification degree, colorless, clear and transparent appearance and low free formaldehyde content, and is matched with a methylene acceptor for use to bond rubber, steel wires and other framework materials. The method overcomes the complex process of synthesizing the methylated melamine formaldehyde resin by an intermittent method, and provides a new method for the research and development of the preparation process of the methylated melamine formaldehyde resin. Therefore, the method has the advantages of avoiding the problem of poor product quality among batches, along with easy operation, good product stability and high yield.
Detailed Description
The invention is further illustrated by the following examples.
Example 1:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: quantitatively adding formaldehyde, melamine and liquid caustic soda into a pipeline, conveying at a constant speed, heating to 60-70 ℃ in the conveying process, and reacting for 10-12 min under heat preservation; in the raw materials, the molar ratio of formaldehyde to melamine is 6.9-7.1, and the PH is controlled to be 8-9;
step 2: after the heat preservation reaction is finished, quantitatively adding methanol into a pipeline flowing at a constant speed, controlling the temperature, adding hydrochloric acid to adjust the pH = 3-4, preserving the heat for 5-7 min, and then quantitatively adding liquid caustic soda to adjust the pH = 8-9; the molar ratio of the melamine to the methanol added into the pipeline is 1; then the reaction system enters a film evaporator to carry out negative pressure distillation to 65-70 ℃;
and 3, step 3: quantitatively adding the semi-finished product subjected to rough steaming and methanol into a pipeline, after controlling the temperature, quantitatively adding hydrochloric acid to adjust the pH = 3-4, reacting for 4-6 min under heat preservation, and then quantitatively adding liquid alkali to adjust the pH = 8-9; the molar ratio of the melamine to the methanol added into the pipeline is 1 to 5; then the reaction system enters a film evaporator to carry out negative pressure distillation to 115-120 ℃, and the product methylated melamine formaldehyde resin is obtained by filtration.
Example 2:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: quantitatively adding formaldehyde, melamine and liquid caustic soda into a pipeline, conveying at a constant speed, heating to 65 ℃ in the conveying process, heating the reaction system by a circulating hot water heating system in the heating process, and carrying out heat preservation reaction for 11min; in the raw materials, the molar ratio of formaldehyde to melamine is 7.0, and the pH is controlled to be 8.5;
step 2: after the heat preservation reaction is finished, quantitatively adding methanol into a pipeline flowing at a constant speed, regulating the pH by adding hydrochloric acid after temperature control, and controlling the temperature of a reaction system by using a warm water heating system and a circulating water cooling system in the temperature control process; keeping the temperature for reaction for 6min, and then quantitatively adding liquid alkali to adjust the pH to be 8.5; methanol is added into the pipeline, and the molar ratio of the melamine to the methanol is 1; then the reaction system enters a film evaporator for negative pressure distillation to 68 ℃;
and step 3: quantitatively adding the semi-finished product after the crude steaming and methanol into a pipeline, quantitatively adding hydrochloric acid after temperature control to adjust the pH =3.5, carrying out heat preservation reaction for 5min, and then quantitatively adding liquid caustic soda to adjust the pH =8.5; methanol is added into the pipeline, and the molar ratio of melamine to methanol is 1; and then the reaction system enters a film evaporator for negative pressure distillation to 117 ℃, and the product methylated melamine formaldehyde resin is obtained by filtering.
In the above step 2 and step 3, the etherification reaction temperature was 40 ℃.
Example 3:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: introducing 100g of melamine into a pipeline according to the feeding speed of 100g/h and 450g of formaldehyde according to the feeding speed of 450g/h, simultaneously quantitatively introducing liquid caustic soda into a feeding hole to adjust the pH = 8-9, immersing the pipeline in hot water at 70 ℃, heating, and carrying out heat preservation reaction;
step 2: after reacting for 11min, quantitatively mixing 406g of methanol with the reaction system, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH to be = 3-4, and after reacting for 6min under the condition of heat preservation, quantitatively adding liquid caustic soda to adjust the pH to be = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the temperature of a distilled semi-product to be 70 ℃;
and 3, step 3: quantitatively mixing the semi-product with 152g of methanol, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH = 3-4, keeping the temperature for reaction for 6min, and quantitatively adding liquid alkali to adjust the pH = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the distillation temperature to be 118 ℃; and after the distillation is finished, filtering the materials in the distillation flask to obtain the methylated melamine formaldehyde resin product. The obtained product is colorless transparent liquid, and the content of the combined formaldehyde is 42.3 percent, the content of the free formaldehyde is 0.15 percent, the heating loss is 0.9 percent and the yield is 95.3 percent through the titration detection.
Example 4:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: introducing 100g of melamine into a pipeline according to the feeding speed of 100g/h and 444g of formaldehyde according to 444g/h, simultaneously quantitatively introducing liquid caustic soda into a feeding hole to adjust the pH = 8-9, immersing the pipeline in hot water at 70 ℃, heating, and carrying out heat preservation reaction;
and 2, step: after reacting for 11min, quantitatively mixing 406g of methanol with the reaction system, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid for regulating the pH = 3-4, and after reacting for 6min under heat preservation, quantitatively adding liquid caustic soda for regulating the pH = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the temperature of a distilled semi-product to be 70 ℃;
and step 3: quantitatively mixing the semi-product with 152g of methanol, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH = 3-4, keeping the temperature for reaction for 6min, and quantitatively adding liquid alkali to adjust the pH = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the distillation temperature to be 118 ℃; and after the distillation is finished, filtering the materials in the distillation flask to obtain the methylated melamine formaldehyde resin product. The obtained product is colorless transparent liquid, and the content of the combined formaldehyde is 42.0 percent and the content of the free formaldehyde is 0.13 percent through the titration method, the heating loss is 0.8 percent, and the yield is 94.9 percent.
Example 5:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: introducing 100g of melamine into a pipeline according to the feeding speed of 100g/h and 457g of formaldehyde according to 457g/h, simultaneously quantitatively introducing liquid caustic soda into a feeding hole to adjust the pH value to be = 8-9, and immersing the pipeline in hot water at 70 ℃ for heating and heat preservation reaction;
step 2: after reacting for 11min, quantitatively mixing 406g of methanol with the reaction system, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH to be = 3-4, and after reacting for 6min under the condition of heat preservation, quantitatively adding liquid caustic soda to adjust the pH to be = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the temperature of a distilled semi-product to be 70 ℃;
and 3, step 3: quantitatively mixing the semi-product with 152g of methanol, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH = 3-4, keeping the temperature for reaction for 6min, and quantitatively adding liquid alkali to adjust the pH = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the distillation temperature to be 118 ℃; and after the distillation is finished, filtering the materials in the distillation flask to obtain the methylated melamine formaldehyde resin product. The obtained product is colorless transparent liquid, and the content of the combined formaldehyde is 42.4 percent and the content of the free formaldehyde is 0.14 percent through the titration method, the heating loss is 0.9 percent, and the yield is 95.6 percent.
Example 6:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: introducing 100g of melamine into a pipeline according to the feeding speed of 100g/h and 450g of formaldehyde according to the feeding speed of 450g/h, simultaneously quantitatively introducing liquid caustic soda into a feeding hole to adjust the pH = 8-9, immersing the pipeline in hot water at 70 ℃, heating, and carrying out heat preservation reaction;
step 2: after reacting for 11min, quantitatively mixing 381g of methanol with a reaction system, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH to be = 3-4, and after reacting for 6min under the condition of heat preservation, quantitatively adding liquid caustic soda to adjust the pH to be = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the temperature of a distilled semi-product to be 70 ℃;
and step 3: quantitatively mixing the semi-product with 152g of methanol, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH = 3-4, keeping the temperature for reaction for 6min, and quantitatively adding liquid alkali to adjust the pH = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the distillation temperature to be 118 ℃; and after the distillation is finished, filtering the materials in the distillation flask to obtain the methylated melamine formaldehyde resin product. The obtained product is colorless transparent liquid, and the content of the combined formaldehyde is 42.0 percent and the content of the free formaldehyde is 0.13 percent through the titration method, the heating loss is 0.8 percent, and the yield is 94.5 percent.
Example 7:
step 1: introducing 100g of melamine into a pipeline according to the feeding speed of 100g/h and 450g of formaldehyde according to the feeding speed of 450g/h, simultaneously quantitatively introducing liquid caustic soda into a feeding hole to adjust the pH = 8-9, immersing the pipeline in hot water at 70 ℃, heating, and carrying out heat preservation reaction;
step 2: after reacting for 11min, quantitatively mixing 406g of methanol with the reaction system, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid for regulating the pH = 3-4, and after reacting for 6min under heat preservation, quantitatively adding liquid caustic soda for regulating the pH = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the temperature of a distilled semi-product to be 70 ℃;
and step 3: quantitatively mixing the semi-product with 178g of methanol, immersing a pipeline in water at 40 ℃ for temperature control, quantitatively adding hydrochloric acid to adjust the pH = 3-4, keeping the temperature for reaction for 6min, and quantitatively adding liquid alkali to adjust the pH = 8-9; entering an evaporator at a constant speed for negative pressure distillation, and controlling the distillation temperature to be 118 ℃; and after the distillation is finished, filtering the materials in the distillation flask to obtain the methylated melamine formaldehyde resin product. The obtained product is colorless transparent liquid, and the content of the combined formaldehyde is 42.9 percent and the content of the free formaldehyde is 0.12 percent through the titration method, the heating loss is 0.8 percent, and the yield is 95.5 percent.
Comparative example 1:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: adding 100g of HMM into 188.3g of methanol, heating to 45 ℃, adjusting the pH of a reaction system to 3-4 by using hydrochloric acid (37%), continuing to perform heat preservation reaction for 1 hour, adjusting the pH of the reaction system to 8-9 by using liquid alkali, and finishing the reaction;
step 2: and transferring the material to a distillation flask for negative pressure distillation, and filtering the material in the distillation flask after the distillation is finished to obtain the product of methylated melamine formaldehyde resin. The obtained product is colorless transparent liquid, and the content of the combined formaldehyde is 42.1 percent, the content of the free formaldehyde is 0.20 percent, the heating loss is 0.8 percent and the yield is 90.5 percent through the titration detection.
The method is an intermittent production process, and the methylated melamine formaldehyde resin is directly synthesized by using an intermediate HMM, although the product quality is good, the process is complicated for drying the HMM, and the formaldehyde obtained by dissipation is difficult to treat in the drying process, so that the production cost of the dried HMM is far higher than that of a wet material HMM. The final production cost is far higher than the cost of directly carrying out the next reaction by using wet materials.
Comparative example 2:
a preparation method of methylated melamine formaldehyde resin comprises the following steps:
step 1: adding 100g of melamine into 450g of formaldehyde, adjusting the pH = 8-9 with liquid alkali, starting stirring and heating; and when the temperature is increased to 75 ℃, keeping the temperature for reaction for 1 hour, and controlling the pH = 8-9 of the reaction system by using liquid alkali in the whole process.
And 2, step: keeping the temperature and reacting for 1 hour; cooling, namely cooling the reaction system to 65 ℃, adding 457g of methanol into the reaction container, controlling the temperature to 45 ℃, adjusting the pH of the reaction system to 3-4 by using hydrochloric acid (37%), continuing to perform heat preservation reaction for 1 hour, adjusting the pH of the reaction system to 8-9 by using liquid alkali, and finishing the reaction;
and step 3: transferring the material to a distillation flask for negative pressure distillation, after the distillation is finished, cooling to 65 ℃, adding 457g of methanol into a reaction container, controlling the temperature to 35 ℃, adjusting the pH of the reaction system to 3-4 by hydrochloric acid (37%), continuing to perform heat preservation reaction for 15 minutes, then adjusting the pH of the reaction system to 8-9 by liquid alkali, and finishing the reaction.
And 4, step 4: transferring the material to a distillation flask for negative pressure distillation, and filtering the material in the distillation flask after the distillation is finished to obtain the methylated melamine formaldehyde resin product. The obtained product is colorless transparent liquid, and the content of combined formaldehyde is 41.9 percent and the content of free formaldehyde is 0.21 percent through the titration detection, the heating loss is 0.8 percent, and the yield is 90.1 percent.
The method is also a batch production process, the intermediate is not treated, and the synthesis is carried out by directly carrying out twice etherification and twice distillation, the quality of the final product of the method is qualified, but the process is complex and the batch production method is used, so that more production equipment is used, and excessive labor cost is brought.
In conclusion, the preparation method of the methylated melamine-formaldehyde resin provided by the invention has the advantages of high automation level, easiness in operation, environmental protection, safety, low cost, good product quality, no batch difference and high yield, and meets the requirements of clean and green production.
Claims (5)
1. A preparation method of methylated melamine formaldehyde resin is characterized by comprising the following steps:
step 1: quantitatively adding formaldehyde, melamine and liquid caustic soda into a pipeline, conveying at a constant speed, heating to 60-70 ℃ in the conveying process, and reacting for 10-12 min under heat preservation; in the raw materials, the molar ratio of formaldehyde to melamine is 6.9-7.1, and the PH is controlled to be 8-9;
step 2: after the heat preservation reaction is finished, quantitatively adding methanol into a pipeline flowing at a constant speed, controlling the temperature, adding hydrochloric acid to adjust the pH = 3-4, preserving the heat for 5-7 min, and then quantitatively adding liquid caustic soda to adjust the pH = 8-9; adding methanol into the pipeline, wherein the mol ratio of melamine to methanol is 1; then the reaction system enters a film evaporator to carry out negative pressure distillation to 65-70 ℃;
and step 3: quantitatively adding the semi-finished product after the crude steaming and methanol into a pipeline, quantitatively adding hydrochloric acid after temperature control to adjust the pH = 3-4, carrying out heat preservation reaction for 4-6 min, and then quantitatively adding liquid caustic soda to adjust the pH = 8-9; adding methanol into the pipeline, wherein the molar ratio of melamine to methanol is 1; then the reaction system enters a film evaporator to carry out negative pressure distillation to 115-120 ℃, and the product methylated melamine formaldehyde resin is obtained by filtration.
2. The method for preparing methylated melamine formaldehyde resin according to claim 1, wherein the hydroxylation reaction temperature in the step 1 is 65 ℃; in the raw materials, the molar ratio of formaldehyde to melamine is 7.0.
3. The method for preparing methylated melamine formaldehyde resin according to claim 1, wherein the temperature rise process of step 1 is carried out by raising the temperature of the reaction system with a circulating hot water temperature rise system.
4. The method for preparing methylated melamine formaldehyde resin according to claim 1, wherein in the temperature control process of step 2, a warm water heating system and a circulating water cooling system are used for controlling the temperature of the reaction system.
5. The method for preparing methylated melamine formaldehyde resin according to claim 1, wherein in the step 2 and the step 3, the etherification reaction temperature is 40 ℃.
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2021
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| GB1530021A (en) * | 1975-02-24 | 1978-10-25 | Basf Ag | Aqueous coating agents |
| CN1910162A (en) * | 2004-01-19 | 2007-02-07 | 巴斯福股份公司 | Continuous method for producing highly methylolated melamine and etherified melamine formaldehyde resins |
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