Method for preparing antimony trioxide coated particles by using brominated epoxy resin

Abstract

The invention relates to the technical field of flame-retardant materials, in particular to a method for preparing antimony trioxide coated particles by using brominated epoxy resin, which comprises the following steps: spraying a polyethylene glycol solution to Sb2O3 powder, and drying to obtain Sb2O3 pretreated powder; 0.5-1% of a silane coupling agent and 0.3-5% of an antioxidant are added into brominated epoxy resin, and the mixture is uniformly stirred and crushed for standby application; injecting acetone accounting for 1 / 3 of the volume of the kneading machine into the kneading machine, then starting the kneading machine, running for ten minutes, and emptying; starting a heating sleeve of the kneading machine until the acetone is completely evaporated; adding the Sb2O3 pretreated powder and brominated epoxy resin into the kneading machine, wherein the mass ratio of the Sb2O3 pretreated powder to the brominated epoxy resin is (45-50): (5-8); starting stirring and heating until coating is completed; and after coating, stopping heating, keeping stirring, and discharging until the temperature is naturally reduced to 60 DEG C or below. According to the scheme, the antimony trioxide powder is coated, so that the particle size is increased, the bulk density is increased, and the dust raising amount is greatly reduced.

Description

Technical Field

[0001] The invention relates to the technical field of flame retardant materials, and in particular to a method for preparing antimony trioxide coated particles by using brominated epoxy resin. Background Art

[0002] Antimony trioxide is an inorganic compound, a white crystalline powder, with a melting point of 655°C and a boiling point of 1550°C. It is mainly used as a pigment, flame retardant, etc.

[0003] Antimony trioxide and resin are added to engineering plastics in a certain proportion. The two work together to achieve a flame retardant effect and are widely used in the field of flame retardant engineering plastics. Antimony trioxide is a white powder with a low bulk density, and the powder is very easy to fly.

[0004] In the prior art, antimony trioxide is usually added separately during the production of engineering plastics. However, this method of use causes antimony trioxide powder to fly up, resulting in significant dust pollution. Summary of the invention

[0005] In order to solve the defects in the prior art, the present invention provides a method for preparing antimony trioxide coated particles using brominated epoxy resin, which is specifically achieved by the following technical scheme: A method for preparing antimony trioxide coated particles using brominated epoxy resin comprises the following steps: Take Sb 2 O 3 1-2% polyethylene glycol by weight of the powder is then dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which is then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treating powders; Add 0.5-1% of silane coupling agent and 0.3-5% of antioxidant to the brominated epoxy resin and stir evenly, then let stand for 1-2 hours; then crush to a particle size of ≤50 μm to obtain pretreated brominated epoxy resin for use; Equipment cleaning: inject acetone that accounts for one third of the volume of the kneader into the kneader, then start the kneader and drain it after running for ten minutes; start the heating jacket of the kneader until the acetone evaporates completely; Coating, adding Sb into the kneader 2 O 3 Pretreated powder and pretreated brominated epoxy resin, Sb 2 O 3The mass ratio of the pretreated powder to the pretreated brominated epoxy resin is (45-50): (5-8); stirring and heating are started until the coating is completed; Cool and discharge. After coating is completed, stop heating and keep stirring until the temperature naturally drops to below 60°C before discharging.

[0006] During the coating process, the rotation speed of the kneader is 300-600 rpm.

[0007] During the coating process, the heating temperature of the kneader is 140°C to 160°C.

[0008] During the coating process, the kneader is operated for 20 to 40 minutes.

[0009] The heating temperature of the kneader during the equipment cleaning process was 60°C.

[0010] The heating time of the kneading machine during the equipment cleaning process is 15 minutes.

[0011] The Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0012] When the material is cooled and discharged, it is passed through an 80-mesh sieve to remove uncoated agglomerated particles.

[0013] The technical solution of the present invention has the following advantages: This solution can greatly reduce the dust generated by antimony trioxide during use by coating the antimony trioxide powder to increase the particle size, increase the bulk density, and greatly reduce the dust generated by antimony trioxide during use. The overall coating rate is greater than 77%.

[0014] Polyethylene glycol was used to 2 O 3 Powder pretreatment can improve Sb 2 O 3 Improve the dispersibility of powder and enhance its compatibility with resin matrix.

[0015] Pretreatment of brominated epoxy resin can enhance its compatibility with subsequent coating materials, improve the wettability and dispersibility of the resin during the mixing process, prevent thermal oxidative degradation of brominated epoxy resin at high temperatures, and enhance the weather resistance of the material. DETAILED DESCRIPTION

[0016] The technical solution of the present invention will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0017] In addition, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0018] The invention provides a method for preparing antimony trioxide coated particles by utilizing brominated epoxy resin.

[0019] Example 1 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0020] Take Sb 2 O 3 1% polyethylene glycol (relative molecular weight 4000) by weight of the powder was then dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which was then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0021] Add 0.5% of the mass of brominated epoxy resin to the brominated epoxy resin, silane coupling agent KH-550, and 0.3% of antioxidant BHT, stir evenly, and then let stand for 1 hour. Then crush to a particle size of ≤50μm to obtain the pretreated brominated epoxy resin for use.

[0022] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0023] Coating, add 45 kg Sb into the kneader 2 O 3 Pre-treat powder, 5 kg pre-treat brominated epoxy resin, start stirring, speed 300 rpm, heat to 140°C, and continue stirring for 20 minutes.

[0024] Cool the material, stop heating, and keep stirring at 300 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0025] Example 2 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0026] Take Sb 2 O3 1.2% of the powder mass of polyethylene glycol (relative molecular weight 4000) was then dissolved in deionized water at a mass ratio of 1:10 to obtain a polyethylene glycol solution, which was sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0027] Add 0.6% of the mass of brominated epoxy resin to the brominated epoxy resin, silane coupling agent KH-550, and 0.4% of antioxidant BHT, stir evenly, and then let stand for 2 hours. Then crush to a particle size of ≤50μm, and obtain the pretreated brominated epoxy resin for use.

[0028] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0029] Coating, add 45 kg Sb into the kneader 2 O 3 Pre-treat powder, 5 kg pre-treat brominated epoxy resin, start stirring, speed 600 rpm, heat to 150°C, and continue stirring for 30 minutes.

[0030] Cool the material, stop heating, and keep stirring at 600 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0031] Example 3 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0032] Take Sb 2 O 3 1.5% polyethylene glycol (relative molecular weight 4000) by weight of the powder was dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which was then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0033] Add 0.8% of the mass of brominated epoxy resin to the silane coupling agent KH-550 and 0.5% of the antioxidant BHT to the brominated epoxy resin and stir evenly, then let it stand for 1.5 hours, and then crush it to a particle size of ≤50μm to obtain the pretreated brominated epoxy resin for use.

[0034] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0035] Coating, add 45 kg Sb into the kneader 2 O 3 Pre-treated powder, 5 kg of pre-treated brominated epoxy resin, start stirring, speed 900 rpm, heat to 160°C, and continue stirring for 40 minutes.

[0036] Cool the material, stop heating, and keep stirring at 900 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0037] Example 4 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0038] Take Sb 2 O 3 2% polyethylene glycol (relative molecular weight 4000) by weight of the powder was dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which was then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0039] Add 1% of the mass of brominated epoxy resin to the brominated epoxy resin, silane coupling agent KH-550, and 0.4% of antioxidant BHT, stir evenly, and then let stand for 1.5 hours. Then crush to a particle size of ≤50μm to obtain the pretreated brominated epoxy resin for use.

[0040] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0041] Coating, add 50 kg Sb into the kneader2 O 3 Pre-treat powder, 5 kg pre-treat brominated epoxy resin, start stirring, turn to 300 rpm, heat to 140°C, and continue stirring for 30 minutes.

[0042] Cool the material, stop heating, and keep stirring at 300 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0043] Example 5 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0044] Take Sb 2 O 3 1.8% polyethylene glycol (relative molecular weight 4000) by weight of the powder was then dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which was then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0045] Add 0.9% of the mass of brominated epoxy resin to the brominated epoxy resin, silane coupling agent KH-550, and 0.3% of antioxidant BHT, stir evenly, and then let stand for 2 hours. Then crush to a particle size of ≤50μm, and obtain the pretreated brominated epoxy resin for use.

[0046] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0047] Coating, add 50 kg Sb into the kneader 2 O 3 Pre-treat powder, 5 kg pre-treat brominated epoxy resin, start stirring, speed 600 rpm, heat to 140°C, and continue stirring for 30 minutes.

[0048] Cool the material, stop heating, and keep stirring at 600 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0049] Example 6 Raw material pretreatment, Sb 2 O 3The powder was passed through a 100-mesh sieve to remove lumps.

[0050] Take Sb 2 O 3 1.7% polyethylene glycol (relative molecular weight 4000) by weight of the powder was then dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which was then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0051] Add 0.7% of the mass of brominated epoxy resin to the brominated epoxy resin, silane coupling agent KH-550, and 0.3% of antioxidant BHT, stir evenly, and then let stand for 2 hours. Then crush to a particle size of ≤50μm, and obtain the pretreated brominated epoxy resin for use.

[0052] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0053] Coating, add 50 kg Sb into the kneader 2 O 3 Pre-treat powder, 5 kg pre-treat brominated epoxy resin, start stirring, speed 900 rpm, heat to 160°C, and continue stirring for 20 minutes.

[0054] Cool the material, stop heating, and keep stirring at 900 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0055] Example 7 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0056] Take Sb 2 O 3 1.5% polyethylene glycol (relative molecular weight 4000) by weight of the powder was dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which was then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0057] Add 0.9% of the mass of brominated epoxy resin to the brominated epoxy resin, silane coupling agent KH-550, and 0.4% of antioxidant BHT, stir evenly, and then let stand for 1.5 hours. Then crush to a particle size of ≤50μm to obtain the pretreated brominated epoxy resin for use.

[0058] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0059] Coating, add 50 kg Sb into the kneader 2 O 3 Pre-treated powder, 8 kg of pre-treated brominated epoxy resin, start stirring, speed 600 rpm, heat to 140°C, and continue stirring for 40 minutes.

[0060] Cool the material, stop heating, and keep stirring at 600 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0061] Example 8 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0062] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0063] Coating, add 50 kg Sb into the kneader 2 O 3 Pre-treat powder, 8 kg pre-treat brominated epoxy resin, start stirring, speed 900 rpm, heat to 150°C, and continue stirring for 20 minutes.

[0064] Cool the material, stop heating, and keep stirring at 900 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0065] Example 9 Raw material pretreatment, Sb 2 O 3 The powder was passed through a 100-mesh sieve to remove lumps.

[0066] Take Sb 2 O 31.8% polyethylene glycol (relative molecular weight 4000) by weight of the powder was then dissolved in deionized water at a weight ratio of 1:10 to obtain a polyethylene glycol solution, which was then sprayed onto the Sb 2 O 3 The powder was then dried at 60 degrees Celsius for 2 hours and then sieved to obtain Sb 2 O 3 Pre-treat the powder.

[0067] Add 0.5% of the mass of brominated epoxy resin to the silane coupling agent KH-550 and 0.4% of the antioxidant BHT to the brominated epoxy resin and stir evenly, then let it stand for 2 hours. Then crush it to a particle size of ≤50μm to obtain the pretreated brominated epoxy resin for use.

[0068] Equipment cleaning: inject acetone that accounts for one third of the kneader's volume into the kneader, then start the kneader, run it at 300rpm for ten minutes, and then drain it; start the kneader's heating jacket, heat it to 60℃, and maintain it for 15 minutes until the acetone evaporates. The waste gas is introduced into the waste gas treatment device.

[0069] Coating, add 50 kg Sb into the kneader 2 O 3 Pre-treat powder, 8 kg pre-treat brominated epoxy resin, start stirring, speed 300 rpm, heat to 150°C, and continue stirring for 20 minutes.

[0070] Cool the material, stop heating, and keep stirring at 300 rpm until the temperature naturally drops to below 60°C before discharging. After discharging, pass through an 80-mesh sieve to remove uncoated agglomerated particles.

[0071] The coverage, dust concentration, bulk density and flame retardancy level of the products prepared in the above embodiments were tested.

[0072] The dust density is based on ISO9096 standard, simulating airflow (5m / s) to raise dust and measure the amount of dust.

[0073] The bulk density is tested using a bulk density meter in accordance with GB / T16913-2008.

[0074] Flame retardant properties are tested according to UL94 standard vertical burning grade Table 1 Statistical table of test results of the embodiment

[0075] The blank group is Sb without coating. 2 O 3 powder.

[0076] Through the above process of the present invention, the dust concentration is reduced by 66.7% to 85%, and the bulk density is increased by 33% to 100%.

[0077] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that the rotation speed of the kneader during the coating process is adjusted to 200 rpm.

[0078] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the rotation speed of the kneader during the coating process is adjusted to 150 rpm.

[0079] Table 2 Comparative test results statistics

[0080] From the data in the above table, we can see that when the speed of the kneading machine is reduced to below 200 rpm during the coating process, the coating rate is greatly reduced. This may be due to the low speed and uneven dispersion of the two materials. Therefore, the minimum speed of the kneading machine should be 200 rpm.

[0081] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.

Claims

1. A method for preparing antimony trioxide coated particles using brominated epoxy resin, characterized in that: The following steps are involved: Take 1-2% polyethylene glycol by mass of Sb2O3 powder, and then dissolve it in deionized water at a mass ratio of 1:10 to obtain a polyethylene glycol solution, spray the polyethylene glycol solution onto the Sb2O3 powder while stirring, and then dry it at 60 degrees Celsius for 2 hours, and then sieve it to obtain Sb2O3 pretreated powder; Add 0.5-1% of silane coupling agent and 0.3-5% of antioxidant to the brominated epoxy resin and stir evenly, then let stand for 1-2 hours; then crush to a particle size of ≤50 μm to obtain pretreated brominated epoxy resin for use; Equipment cleaning: inject acetone that accounts for one third of the volume of the kneader into the kneader, then start the kneader and drain it after running for ten minutes; start the heating jacket of the kneader until the acetone evaporates completely; Coating, adding Sb2O3 pretreated powder and pretreated brominated epoxy resin into a kneader, the mass ratio of Sb2O3 pretreated powder and pretreated brominated epoxy resin being (45-50): (5-8); starting stirring and heating until coating is completed; Cool and discharge. After coating is completed, stop heating and keep stirring until the temperature naturally drops to below 60°C before discharging.

2. The method for preparing antimony trioxide coated particles using brominated epoxy resin according to claim 1, characterized in that: During the coating process, the rotation speed of the kneader is 300-600 rpm.

3. The method for preparing antimony trioxide coated particles using brominated epoxy resin according to claim 1, characterized in that: During the coating process, the heating temperature of the kneader is 140°C to 160°C.

4. The method for preparing antimony trioxide coated particles using brominated epoxy resin according to claim 1, characterized in that: During the coating process, the kneader is operated for 20 to 40 minutes.

5. The method for preparing antimony trioxide coated particles using brominated epoxy resin according to claim 1, characterized in that: The heating temperature of the kneader during the equipment cleaning process was 60°C.

6. The method for preparing antimony trioxide coated particles using brominated epoxy resin according to claim 5, characterized in that: The heating time of the kneading machine during the equipment cleaning process is 15 minutes.

7. The method for preparing antimony trioxide coated particles using brominated epoxy resin according to claim 1, characterized in that: The Sb2O3 powder was sieved through a 100-mesh sieve to remove lumps.

8. The method for preparing antimony trioxide coated particles using brominated epoxy resin according to claim 1, characterized in that: When the material is cooled and discharged, it is passed through an 80-mesh sieve to remove uncoated agglomerated particles.

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