Synthesis Method of UV Polyester Acrylate

Abstract

The present invention discloses a method for synthesizing UV polyester acrylate, which includes the process of feeding phthalic anhydride, acrylic acid, epichlorohydrin, and inhibitor in proportion, then adding part of the catalyst and heating, adding the remaining catalyst in batches, and cooling by passing water for stepwise heating and acid value detection. The present invention has the advantages of simple process flow, short time consumption, high production efficiency, no pollution, and high product quality.

Description

Technical Field

[0001] The present invention relates to the technical field of coating preparation, and more particularly to a method for synthesizing UV polyester acrylate. Background Art

[0002] Polyester acrylate is a common UV oligomer, which is prepared by acrylation of low molecular weight polyester polyol. Polyester acrylate has the advantages of low price, low viscosity, low odor, good flexibility, leveling property and pigment wetting property, etc., so it is widely used in the fields of UV coatings, UV inks and UV photosensitive adhesives. The existing synthesis methods of UV polyester acrylate include the following steps: 1) synthesizing an acid containing -COOH from hydroxyethyl acrylate and phthalic anhydride; 2) synthesizing UV polyester acrylate from the acid containing -COOH and hydroxyethyl acrylate; 3) alkali washing; 4) water washing; 5) adding a desolvent. The existing synthesis method has a long process technical route, which takes 72 hours in total, and the quality of the produced product is not good, and the color of the product is deep; moreover, the environmental treatment required in the production process is difficult. Summary of the Invention

[0003] The technical problem to be solved by the present invention is to provide a method for synthesizing UV polyester acrylate to solve the problems of long production process route and poor product quality, so as to simplify the production process.

[0004] To solve the above technical problems, the technical solutions adopted by the present invention are as follows.

[0005] The method for synthesizing UV polyester acrylate specifically includes the following steps:

[0006] S1: At room temperature, put phthalic anhydride, acrylic acid, epichlorohydrin and inhibitor into the reaction kettle according to the ratio, and prepare a catalyst with a mass fraction nine times that of the inhibitor, and then add 40% of the catalyst; after the feeding is completed, start heating, and stop heating when the temperature reaches 75°C;

[0007] S2: Control the temperature at 75-80°C by means of cooling with water and keep it warm for 0.5 hour;

[0008] S3: Add 10% of the catalyst portion and cool with water, control the temperature at 80-90°C and keep it warm for 0.5 hour;

[0009] S4: Add 10% of the catalyst and cool with water, control the temperature at 90-95°C and keep it warm for 0.5 hour;

[0010] S5: Add 20% of the catalyst in two portions and cool with water, control the temperature at 95°C and keep it warm for 1.0 hour;

[0011] S6: Add 10% of the catalyst and cool down the temperature by adding water. Control the temperature at 95 - 100 °C and keep it warm for 0.5 hours.

[0012] S7: Add the last 10% of the catalyst and cool down the temperature by adding water. Control the temperature at 100 - 105 °C and keep it warm for 0.5 hours. Detect the acid value to be 40 - 50 mgkoH / g.

[0013] S8: Cool down the temperature by adding water and control the temperature at 105 - 110 °C and keep it warm for 0.5 hours.

[0014] S9: Cool down the temperature by adding water and control the temperature at 110 - 115 °C and keep it warm for 0.5 hours.

[0015] S10: Cool down the temperature by adding water and control the temperature at 115 - 117 °C and keep it warm. Monitor the acid value in real time during the warming process. When the acid value reaches 2 - 3 mgkoH / g, the UV polyester acrylate is made.

[0016] Further optimize the technical solution. In step S1, 30 - 40 parts of phthalic anhydride, 15 - 20 parts of acrylic acid, 40 - 50 parts of epichlorohydrin, and 0.02 - 1 part of inhibitor are used.

[0017] Further optimize the technical solution. The inhibitor is p - methoxyphenol.

[0018] Further optimize the technical solution. 30 - 36 parts of phthalic anhydride, 15 - 18 parts of acrylic acid, 42 - 48 parts of epichlorohydrin, and 0.02 - 0.05 part of inhibitor are used.

[0019] Further optimize the technical solution. The catalyst is triethylammonium chloride.

[0020] Due to the adoption of the above technical solution, the technical progress achieved by the present invention is as follows.

[0021] The synthesis method of the UV polyester acrylate provided by the present invention can simultaneously achieve 3 chemical processes in one step: the reaction of acid and epoxy group, the reaction of acid anhydride and -OH, and the reaction of -COOH and epoxy group; the process time is short, only 9 hours in total; no wastewater, no waste residue, and no waste gas are generated during the production process, which is environmentally friendly; the prepared product has stable quality, stable viscosity, and water - white color, and the product quality indexes have very good reproducibility. The present invention has the advantages of simple process flow, short time - consuming, high production efficiency, no pollution, and high product quality. Specific Embodiments

[0022] The present invention will be further described in detail below in combination with specific embodiments.

[0023] The synthesis method of the UV polyester acrylate specifically includes the following steps:

[0024] S1: At room temperature, put 30 - 40 parts of phthalic anhydride, 15 - 20 parts of acrylic acid, 40 - 50 parts of epichlorohydrin, and 0.02 - 1 part of p - methoxyphenol into a reaction kettle, and prepare 0.18 - 9 parts of triethylammonium chloride. Then first add 40% of triethylammonium chloride. After the feeding is completed, start heating. Stop heating when the temperature reaches 75°C.

[0025] S2: Control the temperature at 75 - 80°C by cooling with water and keep it warm for 0.5 hour.

[0026] S3: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 80 - 90°C and keep it warm for 0.5 hour.

[0027] S4: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 90 - 95°C and keep it warm for 0.5 hour.

[0028] S5: Add 20% of triethylammonium chloride in two times: add 10% of triethylammonium chloride every 0.5 hour and cool with water. Control the temperature at 95°C and keep it warm for a total of 1.0 hour.

[0029] S6: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 95 - 100°C and keep it warm for 0.5 hour.

[0030] S7: Add the last 10% of triethylammonium chloride and cool with water. Control the temperature at 100 - 105°C and keep it warm for 0.5 hour. Detect the acid value to be 40 - 50 mgKOH / g.

[0031] S8: Cool with water to control the temperature at 105 - 110°C and keep it warm for 0.5 hour.

[0032] S9: Cool with water to control the temperature at 110 - 115°C and keep it warm for 0.5 hour.

[0033] S10: Cool with water to control the temperature at 115 - 117°C and keep it warm. Monitor the acid value in real - time during the warming process. When the acid value reaches 2 - 3 mgKOH / g, the UV polyester acrylate is made.

[0034] The reactions carried out during the production process of the present invention are as follows:

[0035] 1) Epichlorohydrin + acrylic acid → acrylate (intermediate)

[0036]

[0037] 2) Acrylate (intermediate) + phthalic anhydride → branched - chain carboxylic acid

[0038]

[0039] 3) Branched carboxylic acid + epichlorohydrin → UV acrylate

[0040]

[0041] Example 1:

[0042] S1: At room temperature, put 36 parts of phthalic anhydride, 17.5 parts of acrylic acid, 46 parts of epichlorohydrin, and 0.05 part of p-methoxyphenol into the reaction kettle, and prepare 0.45 part of triethylammonium chloride. Then, first add 40% of triethylammonium chloride, and start heating after the feeding is completed. Stop heating when the temperature reaches 75°C.

[0043] S2: Control the temperature at 75 - 80°C by cooling with water and keep it warm for 0.5 hour.

[0044] S3: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 80 - 90°C and keep it warm for 0.5 hour.

[0045] S4: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 90 - 95°C and keep it warm for 0.5 hour.

[0046] S5: Add 20% of triethylammonium chloride in two portions: add 10% of triethylammonium chloride every 0.5 hour and cool with water. Control the temperature at 95°C and keep it warm for a total of 1.0 hour.

[0047] S6: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 95 - 100°C and keep it warm for 0.5 hour.

[0048] S7: Add the last 10% of triethylammonium chloride and cool with water. Control the temperature at 100 - 105°C and keep it warm for 0.5 hour. The acid value is detected to be 40 mg KOH / g.

[0049] S8: Cool with water to control the temperature at 105 - 110°C and keep it warm for 0.5 hour.

[0050] S9: Cool with water to control the temperature at 110 - 115°C and keep it warm for 0.5 hour.

[0051] S10: Cool with water to control the temperature at 115 - 117°C and keep it warm. Monitor the acid value in real time during the warming process. When the acid value reaches 2 mg KOH / g, prepare UV polyester acrylate.

[0052] Example 2:

[0053] S1: At room temperature, put 40 parts of phthalic anhydride, 15 parts of acrylic acid, 50 parts of epichlorohydrin, and 1 part of p-hydroxyanisole into a reaction kettle, and prepare 9 parts of triethylammonium chloride. Then, first add 40% of triethylammonium chloride. After the feeding is completed, start heating. Stop heating when the temperature reaches 75°C.

[0054] S2: Control the temperature at 75 - 80°C by cooling with water and keep it warm for 0.5 hour.

[0055] S3: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 80 - 90°C and keep it warm for 0.5 hour.

[0056] S4: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 90 - 95°C and keep it warm for 0.5 hour.

[0057] S5: Add 20% of triethylammonium chloride in two portions: add 10% of triethylammonium chloride every 0.5 hour and cool with water. Control the temperature at 95°C and keep it warm for a total of 1.0 hour.

[0058] S6: Add 10% of triethylammonium chloride and cool with water. Control the temperature at 95 - 100°C and keep it warm for 0.5 hour.

[0059] S7: Add the last 10% of triethylammonium chloride and cool with water. Control the temperature at 100 - 105°C and keep it warm for 0.5 hour. Detect that the acid value is 45 mgKOH / g.

[0060] S8: Cool with water to control the temperature at 105 - 110°C and keep it warm for 0.5 hour.

[0061] S9: Cool with water to control the temperature at 110 - 115°C and keep it warm for 0.5 hour.

[0062] S10: Cool with water to control the temperature at 115 - 117°C and keep it warm. Monitor the acid value in real time during the warming process. When the acid value reaches 3 mgKOH / g, prepare UV polyester acrylate.

[0063] Example 3:

[0064] S1: At room temperature, put 30 parts of phthalic anhydride, 20 parts of acrylic acid, 40 parts of epichlorohydrin, and 0.02 part of p-hydroxyanisole into a reaction kettle, and prepare 0.18 part of triethylammonium chloride. Then, first add 40% of triethylammonium chloride. After the feeding is completed, start heating. Stop heating when the temperature reaches 75°C.

[0065] S2: Control the temperature at 75 - 80°C by cooling with water and keep it warm for 0.5 hour.

[0066] S3: Add 10% of triethylammonium chloride and cool down by passing water. Control the temperature at 80 - 90 °C and keep warm for 0.5 hour.

[0067] S4: Add 10% of triethylammonium chloride and cool down by passing water. Control the temperature at 90 - 95 °C and keep warm for 0.5 hour.

[0068] S5: Add 20% of triethylammonium chloride in two portions: add 10% of triethylammonium chloride every 0.5 hour and cool down by passing water. Control the temperature at 95 °C and keep warm for a total of 1.0 hour.

[0069] S6: Add 10% of triethylammonium chloride and cool down by passing water. Control the temperature at 95 - 100 °C and keep warm for 0.5 hour.

[0070] S7: Add the last 10% of triethylammonium chloride and cool down by passing water. Control the temperature at 100 - 105 °C and keep warm for 0.5 hour. Detect the acid value to be 50 mgkoH / g.

[0071] S8: Cool down by passing water and control the temperature at 105 - 110 °C and keep warm for 0.5 hour.

[0072] S9: Cool down by passing water and control the temperature at 110 - 115 °C and keep warm for 0.5 hour.

[0073] S10: Cool down by passing water and control the temperature at 115 - 117 °C and keep warm. Monitor the acid value in real time during the warming process. When the acid value reaches 2 mgkoH / g, produce UV polyester acrylate.

[0074] No water is produced during the production process of the present invention. Therefore, dehydration is not required. On the premise of improving the product stability and viscosity stability, the cost of the raw materials used is reduced. The cost of the existing technical route is 15 yuan per kilogram, and the cost of the present invention is 11 yuan per kilogram, a decrease of 4 yuan. In Examples 1 - 3 of the present invention, UV polyester acrylate with water - white color and very good reproducibility of product quality indicators is produced. The present invention has the advantages of simple process flow, short time - consuming, high production efficiency, no pollution, and high product quality.

Claims

1. Synthesis method of UV polyester acrylate, characterized in that, it specifically includes the following steps: S1: At room temperature, put phthalic anhydride, acrylic acid, epichlorohydrin, and inhibitor into a reaction kettle in proportion, and prepare a catalyst with a mass fraction nine times that of the inhibitor, then add 40% of the catalyst; after feeding, start heating, and stop heating when the temperature reaches 75 °C; S2: Control the temperature at 75 - 80 °C by cooling with water and keep it warm for 0.5 hours; S3: Add 10% of the catalyst and cool with water, control the temperature at 80 - 90 °C, and keep it warm for 0.5 hours; S4: Add 10% of the catalyst and cool with water, control the temperature at 90 - 95 °C, and keep it warm for 0.5 hours; S5: Add 20% of the catalyst in two portions and cool with water, control the temperature at 95 °C, and keep it warm for 1.0 hour; S6: Add 10% of the catalyst and cool with water, control the temperature at 95 - 100 °C, and keep it warm for 0.5 hours; S7: Add the last 10% of the catalyst and cool with water, control the temperature at 100 - 105 °C, and keep it warm for 0.5 hours, and detect the acid value to be 40 - 50 mgkoH / g; S8: Cool with water to control the temperature at 105 - 110 °C and keep it warm for 0.5 hours; S9: Cool with water to control the temperature at 110 - 115 °C and keep it warm for 0.5 hours; S10: Cool with water to control the temperature at 115 - 117 °C and keep it warm. During the warming process, monitor the acid value in real time. When the acid value reaches 2 - 3 mgkoH / g, UV polyester acrylate is made.

2. The synthesis method of UV polyester acrylate according to claim 1, characterized in that: in step S1, 30 - 40 parts of phthalic anhydride, 15 - 20 parts of acrylic acid, 40 - 50 parts of epichlorohydrin, and 0.02 - 1 part of inhibitor are used.

3. The synthesis method of UV polyester acrylate according to claim 2, characterized in that: the inhibitor is p - methoxyphenol.

4. The synthesis method of UV polyester acrylate according to claim 3, characterized in that: 30 - 36 parts of phthalic anhydride, 15 - 18 parts of acrylic acid, 42 - 48 parts of epichlorohydrin, and 0.02 - 0.05 part of inhibitor are used.

5. The synthesis method of UV polyester acrylate according to claim 1, characterized in that: the catalyst is triethylammonium chloride.

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