Water-soluble resin with flame-retardant function and preparation

Abstract

The invention discloses a water-soluble resin with a flame-retardant function and a preparation method thereof. The water-soluble resin is prepared from the following raw materials in parts by weight: 400-500g of flax fatty acid; 200 to 240 g of trimethylolpropane; 25 g to 30 g of trimellitic anhydride; 0.02%-0.04% of a drier; 180 to 200 g of phthalic anhydride; 600 to 680 g of ethylene glycol monobutyl ether; 40-50 g of maleic anhydride, 200-300 parts of dehydrated castor oil fatty acid, and 5-15 parts of a preservative. According to the water-soluble resin with the flame-retardant function and the preparation method thereof, in synthesis of the resin, the formula is more reasonable, fusion with the flame retardant is more stable, silicon tetrachloride which is a byproduct of polycrystalline silicon is used in synthesis, so that the prepared flame retardant is higher in flame-retardant efficiency and more obvious in flame-retardant effect, the preparation process is simplified in the preparation process, and the production cost is reduced. Meanwhile, through a reasonable formula and a preparation process, the prepared resin is small in smell, good in constructability, excellent in leveling property, easy to brush and spray, and beneficial to improving the construction environment and human health.

Description

Technical Field

[0001] The invention relates to the technical field of water-soluble resin preparation, in particular to a water-soluble resin with flame retardant function and its preparation. Background Art

[0002] Water-soluble resin, also known as water-soluble resin, is a type of resin that can be completely dissolved in water. It is usually synthesized from polymer compounds through specific chemical reactions. This resin has the advantages of good water solubility, environmental protection, chemical resistance, etc., so it is widely used in water-based coatings, adhesives, printing inks, coated paper, water treatment agents and other fields. Water-soluble resin can also be used in textile printing and dyeing processing, pharmaceutical packaging, capsules, tablets, electronic product manufacturing and assembly processes and other fields. With the continuous advancement of technology and the continuous growth of market demand, the application prospects of water-soluble resins are very broad.

[0003] The physical and chemical properties of water-soluble resins are similar to those of resins, but also have the characteristics of water. Its formula can vary depending on the required performance and application areas. It is generally made by mixing the main monomer, hydrophilic monomer, initiator, chain transfer agent and other additives in a certain proportion and preparing it through polymerization reaction.

[0004] Therefore, the above method has the following problems in preparation:

[0005] The existing water-soluble resin itself does not have significant flame retardant properties. However, the flame retardant properties of water-soluble resins can generally be improved by adding flame retardants and other functional additives, but the effect is relatively weak, the flame retardant performance is poor, and the water-soluble resin itself has a strong and pungent odor. Summary of the invention

[0006] 1. Technical issues to be solved

[0007] In view of the shortcomings of the prior art, the present invention provides a water-soluble resin with flame retardant function and its preparation, which has the advantages of significant flame retardant effect, high flame retardant performance, small odor, stable synthesis, etc., and solves the problems of poor flame retardant performance, weak effect, and strong and pungent odor.

[0008] (II) Technical solution

[0009] To achieve the above object, the present invention provides the following technical solution: a water-soluble resin with flame retardant function, characterized in that it is composed of the following raw materials in parts by weight:

[0010] 400g-500g of linseed fatty acid; 200g-240g of trimethylolpropane; 25g-30g of trimellitic anhydride; 0.02%-0.04% of drying agent; 180g-200g of phthalic anhydride; 600g-680g of ethylene glycol monobutyl ether; 40g-50g of maleic anhydride, 200-300 parts of dehydrated castor oil fatty acid, 5-15 parts of preservative, 1-10 parts of dispersant, 100-150 parts of polyethylene oxide bisphenol A, 40-60 parts of ethylene glycol monobutyl ether, 220-260 parts of trimethylolpropane, 300-320 parts of isophthalic acid, 1-10 parts of triethylamine, 50-100 parts of titanium dioxide, 100-160 parts of melamine resin, and 10-80 parts of water.

[0011] A method for preparing a water-soluble resin with flame retardant function comprises the following steps:

[0012] Step 1: First, take linseed oil fatty acid, phthalic anhydride, and trimethylolpropane, heat-refining them, cool them after heat-refining, then add maleic anhydride and trimellitic anhydride, heat again, heat-refining to make the acid value reach the standard, and dilute the solution with ethylene glycol monobutyl ether;

[0013] Step 2: then add dehydrated castor oil fatty acid, polyethylene oxide bisphenol A, trimethylolpropane and isophthalic acid into a reaction kettle, heat and raise the temperature to carry out polycondensation reaction, when the acid ester reaches the standard, add preservative, dispersant, ethylene glycol monobutyl ether, triethylamine and water, add titanium dioxide and melamine resin after the reaction is completed, stir and mix evenly, and obtain a water-soluble resin for standby use;

[0014] Step 3, replace the air in the flask with nitrogen, add dioxane and silicon tetrachloride, cool with a cold water bath under stirring to lower the temperature of the reaction system, add 3-dichloro-2-propanol, control the reaction temperature, raise the temperature after the dropwise addition, and then keep the temperature to react;

[0015] Step 4: After the hydrochloric acid gas is released, ethylene glycol is dripped into the four-necked flask, the reaction temperature is controlled, and the temperature is increased after the dripping is completed to react. After the hydrochloric acid gas is released, 3-dichloro-2-propanol is dripped, the reaction temperature is controlled, and the temperature is increased after the dripping is completed, and the reaction is carried out by keeping the temperature;

[0016] Step 5: After the hydrochloric acid gas is released, melamine is added, and the mixture is stirred while keeping warm. The pH value of the solution reaches 5 to 6 as the reaction end point, the reaction system is cooled, and then filtered, and the filtrate is distilled under reduced pressure to remove dioxane and low-boiling-point substances, and then cooled, and petroleum ether is added and stirred for washing, and the mixture is transferred to a separating funnel and allowed to stand for stratification, and the lower layer of the feed liquid is separated, and the petroleum ether is removed by distillation under reduced pressure to obtain the product ethylenediaminetetraacetic acid;

[0017] Step 6: Mix the flame retardant component and small molecule water in a mass ratio of 3:7, then add them into an ultrafine grinder and grind them to 4000-6000 mesh, then grind them to 8000-10000 mesh using an ultrafine horizontal sand mill, finally add a foaming agent, and then add ethylenediaminetetraacetic acid into the resin, stir evenly, and a flame retardant water-soluble resin is obtained.

[0018] Preferably, the flame retardant component is composed of the following raw materials: 20-44.6% aluminum hydroxide; 55-79.5% magnesium hydroxide; 0.2-0.4% calcined kaolin; and 0.2-0.4% sodium carbonate.

[0019] Preferably, the amount of the foaming agent used is 0.2-1 wt% of the total weight of the flame retardant component and the small molecule water.

[0020] Preferably, the stirring in step six is ​​carried out at a temperature of 20 to 50° C. and a speed of 50 rpm for 20 to 30 minutes.

[0021] Preferably, the flask in step three is a four-necked flask, containing 0.7 mol of dioxane, 0.1 mol of silicon tetrachloride, and 0.1 mol of 3-dichloro-2-propanol.

[0022] Preferably, in the step five, 0.01 mol of melamine is used.

[0023] (III) Beneficial effects

[0024] Compared with the prior art, the present invention provides a water-soluble resin with flame retardant function and its preparation, which has the following beneficial effects:

[0025] The water-soluble resin with flame retardant function and its preparation have a more reasonable formula and a more stable fusion with a flame retardant in the synthesis of the resin. Silicon tetrachloride, a byproduct of polycrystalline silicon, is used in the synthesis, so that the flame retardant prepared by the resin has higher flame retardant efficiency and more obvious flame retardant effect. The preparation process is simplified during the preparation process. At the same time, through a reasonable formula and preparation process, the prepared resin has little odor, good construction performance, excellent leveling performance, and is easy to brush and spray, which is beneficial to improving the construction environment and personal health, and also reduces the labor intensity of workers. DETAILED DESCRIPTION

[0027] Embodiment 1:

[0028] Step 1: First, take 400g of linseed oil fatty acid, 180g of phthalic anhydride, and 200g of trimethylolpropane, heat them at 225°C until the acid value is 15mgKOH / g, cool them, add 40g of maleic anhydride and 25g of trimellitic anhydride, heat them again to 180°C, heat them until the acid value is 45mgKOH / g, and dilute the solution with 600g of ethylene glycol monobutyl ether;

[0029] Step 2: then add 200 parts of dehydrated castor oil fatty acid, 100 parts of polyethylene oxide bisphenol A, 220 parts of trimethylolpropane and 300 parts of isophthalic acid into a reactor, heat to 200°C for polycondensation reaction, when the acid ester reaches 30, add 5 parts of preservative, 1 part of dispersant, 40 parts of ethylene glycol monobutyl ether, 1 part of triethylamine and 10 parts of water, add 50 parts of titanium dioxide and 100 parts of melamine resin after the reaction is completed, stir and mix evenly to obtain a water-soluble resin for standby use;

[0030] Step 3: In a flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser and a drying tube at the top of the condenser, replace the air in the bottle with nitrogen, add 0.7 mol of dioxane and 0.1 mol of silicon tetrachloride, and cool with a cold water bath under stirring to reduce the temperature of the reaction system to below 25°C, add 0.1 mol of 3-dichloro-2-propanol dropwise, control the reaction temperature not higher than 35°C, raise the temperature to 45°C after the dropwise addition, and keep the reaction for 2h;

[0031] Step 4: After the hydrochloric acid gas is released, 0.05 mol of ethylene glycol is dripped into the four-necked flask, the reaction temperature is controlled not to be higher than 55°C, the temperature is raised to 70°C after the dripping is completed, and the reaction is carried out for 5 hours. After the hydrochloric acid gas is released, 0.22 mol of 3-dichloro-2-propanol is dripped, the reaction temperature is controlled not to be higher than 75°C, the temperature is raised to 80°C after the dripping is completed, and the reaction is kept warm for 7 hours;

[0032] Step 5: After the hydrochloric acid gas is released, 0.01 mol of melamine is added, and the mixture is stirred for 1 hour at a temperature of 5. The pH value of the solution is taken as the reaction end point, and the reaction system is cooled to 30°C, filtered, and the filtrate is distilled under reduced pressure to remove dioxane and low-boiling-point substances, and then cooled to 60°C, and petroleum ether is added and stirred for washing, and the mixture is transferred to a separating funnel and allowed to stand for stratification, and the lower layer of the feed liquid is separated, and the petroleum ether is removed by distillation under reduced pressure to obtain the product ethylenediaminetetraacetic acid;

[0033] Step six, 20% aluminum hydroxide, 55% magnesium hydroxide, 0.2% calcined kaolin and 0.2% sodium carbonate are mixed in a mass ratio of 3:7, then added to an ultrafine grinder and ground to 4000 mesh, and then ground to 8000 mesh by an ultrafine horizontal sand mill, and finally 0.2wt% of a foaming agent is added, and then ethylenediaminetetraacetic acid is added to the interior of the resin, the temperature is controlled at 20°C, and stirred at 50 rpm for 20 minutes to obtain a flame retardant water-soluble resin.

[0034] Embodiment 2:

[0035] Step 1: First, take 500g of linseed oil fatty acid, 200g of phthalic anhydride, and 240g of trimethylolpropane, heat them at 225°C until the acid value is 15mgKOH / g, cool them, add 50g of maleic anhydride and 30g of trimellitic anhydride, heat them again to 180°C, heat them until the acid value is 45mgKOH / g, and dilute the solution with 680g of ethylene glycol monobutyl ether;

[0036] Step 2: 300 parts of dehydrated castor oil fatty acid, 150 parts of polyethylene oxide bisphenol A, 260 parts of trimethylolpropane and 320 parts of isophthalic acid are added into a reaction kettle, and the temperature is raised to 200° C. for polycondensation reaction. When the acid ester reaches 30, 15 parts of preservative, 10 parts of dispersant, 60 parts of ethylene glycol monobutyl ether, 10 parts of triethylamine and 80 parts of water are added. After the reaction is completed, 100 parts of titanium dioxide and 160 parts of melamine resin are added, and the mixture is stirred and mixed to obtain a water-soluble resin for use;

[0037] Step 3: In a flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser and a drying tube at the top of the condenser, replace the air in the bottle with nitrogen, add 0.7 mol of dioxane and 0.1 mol of silicon tetrachloride, and cool with a cold water bath under stirring to reduce the temperature of the reaction system to below 25°C, add 0.1 mol of 3-dichloro-2-propanol dropwise, control the reaction temperature not higher than 35°C, raise the temperature to 45°C after the dropwise addition, and keep the reaction for 2h;

[0038] Step 4: After the hydrochloric acid gas is released, 0.05 mol of ethylene glycol is dripped into the four-necked flask, the reaction temperature is controlled not to be higher than 55°C, the temperature is raised to 70°C after the dripping is completed, and the reaction is carried out for 5 hours. After the hydrochloric acid gas is released, 0.22 mol of 1,3-dichloro-2-propanol is dripped, the reaction temperature is controlled not to be higher than 75°C, the temperature is raised to 80°C after the dripping is completed, and the reaction is kept warm for 7 hours;

[0039] Step 5: After the hydrochloric acid gas is released, add 0.01 mol of melamine, keep warm and stir for 1 hour, and take the pH value of the solution as 6 as the reaction end point, cool the reaction system to 30°C, filter, and distill the filtrate under reduced pressure to remove dioxane and low-boiling substances, then cool to 60°C, add petroleum ether, stir and wash, transfer to a separating funnel, stand and separate, separate the lower layer of feed liquid, and distill under reduced pressure to remove petroleum ether to obtain the product ethylenediaminetetraacetic acid;

[0040] Step six, 44.6% aluminum hydroxide, 79.5% magnesium hydroxide, 0.4% calcined kaolin and 0.4% sodium carbonate are mixed in a mass ratio of 3:7, then added to an ultrafine grinder and ground to 6000 mesh, and then ground to 10000 mesh by an ultrafine horizontal sand mill, and finally a foaming agent is added, and then ethylenediaminetetraacetic acid is added to the interior of the resin, the temperature is controlled at 50°C, and stirred at 50 rpm for 30 minutes to obtain a flame retardant water-soluble resin.

[0041] The beneficial effects of the present invention are as follows: the water-soluble resin with flame retardant function and its preparation have a more reasonable formula and a more stable fusion with the flame retardant in the synthesis of the resin, and silicon tetrachloride, a byproduct of polycrystalline silicon, is used in the synthesis, so that the flame retardant prepared by the resin has higher flame retardant efficiency and more obvious flame retardant effect, and the preparation process is simplified during the preparation process. At the same time, through a reasonable formula and preparation process, the prepared resin has a small odor, good construction performance, excellent leveling performance, and is easy to brush and spray, which is beneficial to improving the construction environment and personal health, and also reduces the labor intensity of the staff.

[0042] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A water-soluble resin with flame retardant function, characterized in that: The composition is composed of the following raw materials in parts by weight: 400g-500g of linseed fatty acid; 200g-240g of trimethylolpropane; 25g-30g of trimellitic anhydride; 0.02%-0.04% of drying agent; 180g-200g of phthalic anhydride; 600g-680g of ethylene glycol monobutyl ether; 40g-50g of maleic anhydride, 200-300 parts of dehydrated castor oil fatty acid, 5-15 parts of preservative, 1-10 parts of dispersant, 100-150 parts of polyethylene oxide bisphenol A, 40-60 parts of ethylene glycol monobutyl ether, 220-260 parts of trimethylolpropane, 300-320 parts of isophthalic acid, 1-10 parts of triethylamine, 50-100 parts of titanium dioxide, 100-160 parts of melamine resin, and 10-80 parts of water.

2. The water-soluble resin with flame retardant function according to claim 1, characterized in that: The preparation process includes the following steps: Step 1: First, take linseed oil fatty acid, phthalic anhydride, and trimethylolpropane, heat-refining them, cool them after heat-refining, then add maleic anhydride and trimellitic anhydride, heat again, heat-refining to make the acid value reach the standard, and dilute the solution with ethylene glycol monobutyl ether; Step 2: then add dehydrated castor oil fatty acid, polyethylene oxide bisphenol A, trimethylolpropane and isophthalic acid into a reaction kettle, heat and raise the temperature to carry out polycondensation reaction, when the acid ester reaches the standard, add preservative, dispersant, ethylene glycol monobutyl ether, triethylamine and water, add titanium dioxide and melamine resin after the reaction is completed, stir and mix evenly, and obtain a water-soluble resin for standby use; Step 3, replace the air in the flask with nitrogen, add dioxane and silicon tetrachloride, cool with a cold water bath under stirring to lower the temperature of the reaction system, add 3-dichloro-2-propanol, control the reaction temperature, raise the temperature after the dropwise addition, and then keep the temperature to react; Step 4: After the hydrochloric acid gas is released, ethylene glycol is dripped into the four-necked flask, the reaction temperature is controlled, and the temperature is increased after the dripping is completed to react. After the hydrochloric acid gas is released, 3-dichloro-2-propanol is dripped, the reaction temperature is controlled, and the temperature is increased after the dripping is completed, and the reaction is carried out by keeping the temperature; Step 5: After the hydrochloric acid gas is released, melamine is added, and the mixture is stirred while keeping warm. The pH value of the solution reaches 5 to 6 as the reaction end point, the reaction system is cooled, and then filtered, and the filtrate is distilled under reduced pressure to remove dioxane and low-boiling-point substances, and then cooled, and petroleum ether is added and stirred for washing, and the mixture is transferred to a separating funnel and allowed to stand for stratification, and the lower layer of the feed liquid is separated, and the petroleum ether is removed by distillation under reduced pressure to obtain the product ethylenediaminetetraacetic acid; Step 6: Mix the flame retardant component and small molecule water in a mass ratio of 3:7, then add them into an ultrafine grinder and grind them to 4000-6000 mesh, then grind them to 8000-10000 mesh using an ultrafine horizontal sand mill, finally add a foaming agent, and then add ethylenediaminetetraacetic acid into the resin, stir evenly, and a flame retardant water-soluble resin is obtained.

3. The water-soluble resin with flame retardant function according to claim 2, characterized in that: The flame retardant component is composed of the following raw materials: 20-44.6% of aluminum hydroxide; 55-79.5% of magnesium hydroxide; 0.2-0.4% of calcined kaolin; and 0.2-0.4% of sodium carbonate.

4. The water-soluble resin with flame retardant function according to claim 2, characterized in that: The amount of the foaming agent used is 0.2-1 wt% of the total weight of the flame retardant component and the small molecule water.

5. The water-soluble resin with flame retardant function according to claim 2, characterized in that: In the step 6, the stirring is carried out at a temperature of 20 to 50° C. and a speed of 50 rpm for 20 to 30 minutes.

6. The water-soluble resin with flame retardant function according to claim 2, characterized in that: In the step 3, 0.7 mol of dioxane, 0.1 mol of silicon tetrachloride, and 0.1 mol of 3-dichloro-2-propanol are added, and the flask is a four-necked flask.

7. The water-soluble resin with flame retardant function according to claim 2, characterized in that: In the step 5, 0.01 mol of melamine is used.