CN115260595B - Anti-yellowing heat-conducting flame retardant and preparation method thereof - Google Patents
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Abstract
The invention provides an anti-yellowing heat-conducting flame retardant and a preparation method thereof, wherein the preparation method comprises the following steps: s1, dissolving magnesium salt and aluminum salt in water, adding a complexing agent to form xerogel, calcining and grinding to obtain Al-Mg oxide micro powder; s2, dispersing the Al-Mg oxide micro powder in water, adding a catalyst and dopamine hydrochloride, heating, stirring, reacting, centrifuging, and washing to obtain polydopamine/Al-Mg oxide micro powder; s3, adding the organic flame retardant solution into the polydopamine/Al-Mg oxide micro powder prepared in the step S2, uniformly dispersing, stirring for reaction, centrifuging, and drying to obtain the anti-yellowing heat-conducting flame retardant. The flame retardant plastic prepared by the invention has excellent flame retardant property, heat conductive property and yellowing resistance.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to an anti-yellowing heat-conducting flame retardant and a preparation method thereof.
Background
The flame retardant is widely applied to high polymer materials. Flame retardants are classified into halogen-containing flame retardants and halogen-free flame retardants. The halogen-containing flame retardant has the advantages of small addition amount, good flame retardant effect stability and the like, but also has the problems of secondary hazard and potential environmental influence caused by a large amount of smoke and toxic corrosive hydrogen halide gas generated after combustion. The halogen-free flame retardant mainly comprises phosphorus-nitrogen compounds and metal hydroxide. The smoke generating agent has the advantages of small smoke generating amount during combustion and no generation of toxic and harmful gas, but also has the problems of large addition amount and easy precipitation and migration. Wherein magnesium hydroxide is a filled flame retardant, which releases bound water when decomposed by heat to absorb a large amount of latent heat, thereby lowering the surface temperature of the synthetic material filled with the magnesium hydroxide in flame, and has the effects of inhibiting polymer decomposition and cooling the generated combustible gas.
Bromine-containing flame retardants are limited in application in some fields in recent years due to environmental protection, but are main flame retardants in the current market due to mature production process, low cost and good flame retardant effect. In order to exert the respective advantages of halogen-containing and halogen-free flame retardants, the use of flame retardants for compounding has been a hot spot of research. Another disadvantage of bromine flame retardants is the tendency to yellowing when applied in engineering plastics. The research and development of the flame retardant with excellent yellowing resistance and heat conductivity has important significance
The existing flame retardant has flame retardant effect only, and when the flame retardant is added into a polymer substrate to prepare heat-conducting plastic, the heat-conducting plastic is difficult to simultaneously have heat-conducting performance, so that the dual requirements of the current heat-conducting plastic field on heat conduction and flame retardance cannot be met. Meanwhile, the addition of the flame retardant has a certain influence on the mechanical properties of the material. .
Disclosure of Invention
The invention aims to provide a preparation method of an anti-yellowing heat-conducting flame retardant, which takes Al-Mg oxide as a core, and a layer of flame retardant molecules is loaded on the surface of the flame-retardant, so that the flame-retardant plastic has excellent flame retardant property, good heat-conducting property and good dispersion in plastics, and the mechanical properties of the plastics are not greatly influenced, and the prepared flame-retardant plastic has excellent flame retardant property, heat-conducting property and anti-yellowing property.
The technical scheme of the invention is realized as follows:
the preparation method of the anti-yellowing heat-conducting flame retardant comprises the following steps:
s1, dissolving magnesium salt and aluminum salt in water, adding a complexing agent, heating to 55-65 ℃ and evaporating a solvent to obtain sol; then the temperature is increased to 140-170 ℃, the vacuum degree is reduced to 0.01-0.1MPa, xerogel is formed, the calcination is carried out for 2-4 hours at 500-600 ℃, and the powder is ground to obtain Al-Mg oxide micro powder;
s2, dispersing the Al-Mg oxide micro powder prepared in the step S1 in water, adding a catalyst and dopamine hydrochloride, heating, stirring, reacting, centrifuging, and washing with water to obtain polydopamine/Al-Mg oxide micro powder;
s3, adding the organic flame retardant composition into an organic solvent, adding the polydopamine/Al-Mg oxide micro powder prepared in the step S2, uniformly dispersing, stirring for reaction, centrifuging, and drying to obtain the anti-yellowing heat-conducting flame retardant.
As a further improvement of the invention, the magnesium salt in step S1 is selected from at least one of magnesium nitrate, magnesium sulfate, magnesium chloride; the aluminum salt is at least one selected from aluminum nitrate, aluminum chloride and aluminum sulfate; the complexing agent is a composition of a polycarboxylic acid complexing agent and a trialkanolamine, and the polycarboxylic acid complexing agent is at least one of citric acid or sodium citrate; the triol amine complexing agent is at least one selected from triethanolamine and tripropanolamine.
Preferably, the complexing agent is the combination of citric acid and triethanolamine, and the mass ratio is 3:1-3.
As a further improvement of the invention, the mass ratio of the magnesium salt, the aluminum salt and the complexing agent in the step S1 is 1-2:3-5:7-12.
Further, the grain size of the Al-Mg oxide micro powder obtained in the step S1 is 400-800nm.
As a further improvement of the invention, the catalyst in the step S2 is Tris-HCl solution with pH of 5.5-6.5, the temperature is heated to 35-40 ℃, and the reaction time is 3-5h.
As a further improvement of the invention, the mass ratio of the Al-Mg oxide micro powder to the dopamine hydrochloride in the step S2 is 5-10:2.5-4.
As a further improvement of the present invention, the organic flame retardant composition in step S3 is selected from the group consisting of a bromine-containing flame retardant selected from decabromodiphenylethane, bromotriazine, octabromoether, methyl octabromoether, and a melamine flame retardant; the melamine flame retardant is at least one selected from melamine polyphosphate and melamine cyanurate.
Preferably, the mass ratio of the bromine-containing flame retardant to the melamine flame retardant is 3-5:1, more preferably, the organic flame retardant is a compound of bromotriazine and melamine cyanurate according to the mass ratio of 3-5:1.
Preferably, the organic solvent is selected from at least one of dichloromethane, dichloroethane, chloroform and carbon tetrachloride.
As a further improvement of the invention, the mass ratio of the organic flame retardant composition to the polydopamine/Al-Mg oxide micro powder in the step S3 is 3-5:10, and the reaction time is 1-3h.
The invention further protects the anti-yellowing heat-conducting flame retardant prepared by the preparation method.
The invention further protects a flame-retardant engineering plastic, which comprises the anti-yellowing heat-conducting flame retardant, wherein the mass of the flame-retardant engineering plastic accounts for 10-20%, preferably 12-16%; examples of such engineering plastics include, but are not limited to, polyesters, nylons, polycarbonates, polyimides, polyphenylene sulfides, polysulfones, polyamides, polyaryletherketones.
The invention has the following beneficial effects:
the invention prepares Al-Mg oxide micro powder by sol-gel method, adds complexing agent into solution containing aluminum salt and magnesium salt to form metal-citric acid (sodium) reaction system, citric acid is weak acid, takes multi-stage dissociating reaction, and adds metal ion Al into metal ion Al 3+ Or Mg (Mg) 2+ Forming a complex in the presence of the catalyst; triethanolamine is also capable of complexing with metal ions. The two complexing agents are used together to improve the gel morphology, so that Mg and Al are dispersed in the gel more uniformly, and the flame retardant property and the heat conducting property are improved.
The temperature is increased, the pressure is reduced, xerogel is obtained, the xerogel is calcined, al-Mg oxide micro powder is obtained, the surface of the Al-Mg oxide micro powder is further coated with a polydopamine layer, polydopamine is rich in active groups such as hydroxyl, amino, carboxyl and the like, and can form hydrogen bonds with oxygen atoms, ammonia atoms and the like on organic flame retardant molecules, so that stable complexes are formed, and the flame retardant is fixed.
The invention adopts a compound complex, which comprises a polycarboxylic acid complexing agent and an alcohol amine complexing agent, and can stably fix Al ions and Mg ions through carboxylate radicals, amino groups and hydroxyl groups, thereby obtaining stable gel. The inventor finds that under the action of the compounded complexing agent, the obtained Al-Mg oxide micro powder has better dispersion uniformity, and the Al-Mg oxide micro powder prepared by a single complexing agent has uneven dispersion, is easy to adhere and has reduced flame retardant property.
The invention takes Al-Mg oxide as a core, and a layer of flame retardant molecules is loaded on the surface, so that the flame retardant plastic has excellent flame retardant property and heat conducting property, and the nano structure of the flame retardant plastic can be beneficial to dispersing in the plastic, so that the mechanical property of the plastic is not greatly influenced, and the prepared flame retardant plastic has excellent flame retardant property.
In the flame retardant, the brominated flame retardant is stably anchored on the polydopamine/Al-Mg oxide micro powder, and can play an obvious anti-yellowing role.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is an SEM image of fine powder of Al-Mg oxide obtained in example 1.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a preparation method of an anti-yellowing heat-conducting flame retardant, which comprises the following steps:
s1, dissolving 1 part by weight of magnesium sulfate and 3 parts by weight of aluminum sulfate in 100 parts by weight of water, adding 7 parts by weight of complexing agent, heating to 55 ℃ and evaporating a solvent to obtain sol; then the temperature is increased to 140 ℃, the vacuum degree is reduced to 0.01MPa, xerogel is formed, the xerogel is taken out, calcined for 2 hours at 500 ℃, ground and sieved by a 500-mesh sieve, and the Al-Mg oxide micro powder is obtained; the complexing agent is a compound mixture of sodium citrate and triethanolamine, and the mass ratio is 3:1.
FIG. 1 is an SEM image of the obtained Al-Mg oxide fine powder, and it is understood that the obtained Al-Mg oxide fine powder has a uniform particle size distribution, no blocking, and a particle size of 400-800nm.
S2, dispersing 5 parts by weight of the Al-Mg oxide micro powder prepared in the step S1 into 20 parts by weight of Tris-HCl solution with the pH of 5.5, adding 2.5 parts by weight of dopamine hydrochloride, heating to 35 ℃, stirring and reacting for 3h, centrifuging for 15min at 3000r/min, and alternately washing with water and ethanol for three times to obtain polydopamine coated Al-Mg oxide micro powder;
s3, adding 3 parts by weight of the organic flame retardant composition into 50 parts by weight of dichloromethane, adding 10 parts by weight of the polydopamine coated Al-Mg oxide micro powder prepared in the step S2, uniformly dispersing, stirring and reacting for 1h, and evaporating the solvent to obtain the anti-yellowing heat-conducting flame retardant.
The organic flame retardant composition is a compound mixture of bromotriazine and melamine cyanurate, and the mass ratio is 3:1.
Example 2
The embodiment provides a preparation method of an anti-yellowing heat-conducting flame retardant, which comprises the following steps:
s1, dissolving 2 parts by weight of magnesium chloride and 5 parts by weight of aluminum chloride in 100 parts by weight of water, adding 12 parts by weight of complexing agent, heating to 65 ℃ and evaporating the solvent to obtain sol; then the temperature is increased to 170 ℃, the vacuum degree is reduced to 0.1MPa, xerogel is formed, the xerogel is taken out, calcined for 4 hours at 600 ℃, ground and sieved by a 500-mesh sieve, and the Al-Mg oxide micro powder is obtained; the complexing agent is a compound mixture of sodium citrate and triethanolamine, and the mass ratio is 1:1.
S2, dispersing 5 parts by weight of the Al-Mg oxide micro powder prepared in the step S1 in water, adding 1.5 parts by weight of Tris-HCl solution with pH of 6.5 and 4 parts by weight of dopamine hydrochloride, heating to 40 ℃, stirring and reacting for 5 hours, centrifuging for 15 minutes 3000r/min, and washing with water to obtain polydopamine/Al-Mg oxide micro powder;
s3, adding 5 parts by weight of the organic flame retardant composition into 50 parts by weight of chloroform, adding 10 parts by weight of the polydopamine/Al-Mg oxide micro powder prepared in the step S2, uniformly dispersing, stirring and reacting for 3 hours, and evaporating the solvent to obtain the anti-yellowing heat-conducting flame retardant.
The organic flame retardant composition is a compound mixture of bromotriazine and melamine cyanurate, and the mass ratio is 5:1.
Example 3
The embodiment provides a preparation method of an anti-yellowing heat-conducting flame retardant, which comprises the following steps:
s1, dissolving 1.5 parts by weight of magnesium nitrate and 4 parts by weight of aluminum nitrate in 100 parts by weight of water, adding 10 parts by weight of complexing agent, heating to 60 ℃ and evaporating the solvent to obtain sol; then the temperature is increased to 165 ℃, the vacuum degree is reduced to 0.05MPa, xerogel is formed, the xerogel is taken out, calcined for 3 hours at 550 ℃, ground and sieved by a 500-mesh sieve, and the Al-Mg oxide micro powder is obtained;
the complexing agent is a compound mixture of sodium citrate and triethanolamine, and the mass ratio is 3:2.
S2, dispersing 5 parts by weight of the Al-Mg oxide micro powder prepared in the step S1 in water, adding 1.5 parts by weight of Tris-HCl solution with pH of 6 and 3.3 parts by weight of dopamine hydrochloride, heating to 37 ℃, stirring and reacting for 4 hours, centrifuging for 15 minutes at 3000r/min, and washing with water to obtain polydopamine/Al-Mg oxide micro powder;
s3, adding 4 parts by weight of the organic flame retardant composition into 50 parts by weight of dichloromethane, adding 10 parts by weight of the polydopamine/Al-Mg oxide micro powder prepared in the step S2, uniformly dispersing, stirring and reacting for 2 hours, and evaporating the solvent to obtain the anti-yellowing heat-conducting flame retardant.
The organic flame retardant composition is a compound mixture of bromotriazine and melamine cyanurate, and the mass ratio is 4:1.
Example 4
In contrast to example 3, the complexing agent was a single triethanolamine, with no other conditions changed.
Example 5
In contrast to example 3, the complexing agent was sodium citrate alone, with no other conditions being altered.
Application example
The heat-conducting flame-retardant plastic is obtained by mixing the following raw materials according to the proportion of the raw materials, and carrying out melt extrusion granulation.
100 parts of PA66 resin (purchased from Guangzhou Xinsheng engineering plastics Co., ltd., product No. EPR 27), 15 parts of flame retardant prepared in the example, 2 parts of polyethylene wax, 3 parts of Exxon Mobil POE elastomer (trade mark 9371), 1 part of opacifier titanium dioxide and 7 parts of silicon carbide. The following performance tests were carried out on the obtained flame retardant plastic, and the results are shown in table 1.
Comparative example 1
100 parts of PA66 resin (EPR 27), 5.2 parts of flame retardant (a compound mixture of bromotriazine and melamine cyanurate according to a mass ratio of 4:1), 2.2 parts of magnesium hydroxide, 4.5 parts of aluminum hydroxide, 2 parts of polyethylene wax, 3 parts of Exxon Mobil POE elastomer (trade mark 9371), 1 part of opacifier titanium dioxide and 7 parts of silicon carbide. The following performance tests were carried out on the obtained flame retardant plastic, and the results are shown in table 1.
The thermal conductivity is determined by reference to the method described in GB/T3399-1982.
Tensile strength was determined by the method of GB/T1040.2-2006.
Flexural strength was determined by reference to GB/T9341-2008 method.
The yellowing resistance is measured by a wind-light-breadth color difference meter according to the method in GB/T16422.2-2014, and the yellowing index delta YI before and after irradiation is measured by irradiating for 480 hours in a xenon lamp exposure light yellowing test box.
TABLE 1 flame retardant engineering plastics Properties
As shown in the table above, the plastic prepared by adding the anti-yellowing heat-conducting flame retardant prepared by the embodiment of the invention into the plastic composition has good mechanical properties, obviously improved heat conductivity and flame retardance and good anti-yellowing property. Examples 4 and 5 used either triethanolamine alone or sodium citrate as the complexing agent, and the resulting nylon engineering plastic had a reduced thermal conductivity and limiting oxygen index. The possible reason is that the adoption of the compounded complexing agent can improve the dispersion condition of the flame retardant, thereby improving the heat conductivity and flame retardance of the flame retardant.
Claims (13)
1. The preparation method of the anti-yellowing heat-conducting flame retardant comprises the following steps:
s1, dissolving magnesium salt and aluminum salt in water, adding a complexing agent, heating to 55-65 ℃ and evaporating a solvent to obtain sol; then the temperature is increased to 140-170 ℃, the vacuum degree is reduced to 0.01-0.1MPa, xerogel is formed, the calcination is carried out for 2-4 hours at 500-600 ℃, and the powder is ground to obtain Al-Mg oxide micro powder;
s2, dispersing the Al-Mg oxide micro powder prepared in the step S1 in water, adding a catalyst and dopamine hydrochloride, heating, stirring, reacting, centrifuging, and washing with water to obtain polydopamine/Al-Mg oxide micro powder;
s3, adding the organic flame retardant composition into an organic solvent, adding the polydopamine/Al-Mg oxide micro powder prepared in the step S2, uniformly dispersing, stirring for reaction, centrifuging, and drying to obtain the anti-yellowing heat-conducting flame retardant.
2. The method according to claim 1, wherein the magnesium salt in step S1 is at least one selected from the group consisting of magnesium nitrate, magnesium sulfate and magnesium chloride; the aluminum salt is at least one selected from aluminum nitrate, aluminum chloride and aluminum sulfate; the complexing agent is a composition of a polycarboxylic acid complexing agent and a trialkanolamine, and the polycarboxylic acid complexing agent is at least one of citric acid or sodium citrate; the triol amine complexing agent is at least one selected from triethanolamine and tripropanolamine.
3. The preparation method of claim 1, wherein the complexing agent in step S1 is a combination of citric acid and triethanolamine in a mass ratio of 3:1-3.
4. The method according to claim 3, wherein the mass ratio of the magnesium salt, the aluminum salt and the complexing agent in the step S1 is 1-2:3-5:7-12.
5. The preparation method according to claim 1, wherein the particle size of the Al-Mg oxide fine powder obtained in the step S1 is 400-800nm.
6. The preparation method according to claim 1, wherein the catalyst in the step S2 is Tris-HCl solution with pH of 5.5-6.5, and the catalyst is heated to 35-40 ℃ for 3-5h.
7. The preparation method according to claim 1, wherein the mass ratio of the Al-Mg oxide fine powder to the dopamine hydrochloride in the step S2 is 5-10:2.5-4.
8. The method of claim 1, wherein the organic flame retardant composition in step S3 is selected from the group consisting of a bromine-containing flame retardant selected from decabromodiphenylethane, bromotriazine, octabromoether, methyl octabromoether, and a melamine flame retardant; the melamine flame retardant is at least one selected from melamine polyphosphate and melamine cyanurate.
9. The preparation method of claim 8, wherein the organic flame retardant is a compound of bromotriazine and melamine cyanurate according to a mass ratio of 3-5:1.
10. The preparation method according to claim 1, wherein the mass ratio of the organic flame retardant composition to the polydopamine/Al-Mg oxide micro powder in the step S3 is 3-5:10, and the reaction time is 1-3h.
11. An anti-yellowing heat-conducting flame retardant prepared by the preparation method of any one of claims 1 to 10.
12. A flame-retardant engineering plastic, comprising the anti-yellowing heat-conducting flame retardant according to claim 11, wherein the mass of the flame-retardant engineering plastic accounts for 10-20% of the mass of the flame-retardant engineering plastic; the engineering plastic comprises polyester, nylon, polycarbonate, polyimide, polyphenylene sulfide, polysulfone, polyamide or polyaryletherketone.
13. The flame-retardant engineering plastic according to claim 12, wherein the anti-yellowing heat-conducting flame retardant accounts for 12-16% of the mass of the flame-retardant engineering plastic.
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| CN107457858A (en) * | 2017-08-30 | 2017-12-12 | 常州市天宁区鑫发织造有限公司 | A kind of particieboard fire retardant |
| CN114213850A (en) * | 2021-12-28 | 2022-03-22 | 江苏达胜高聚物股份有限公司 | High-thermal-conductivity silicone rubber cable material and preparation method and application thereof |
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| CN107457858A (en) * | 2017-08-30 | 2017-12-12 | 常州市天宁区鑫发织造有限公司 | A kind of particieboard fire retardant |
| CN114213850A (en) * | 2021-12-28 | 2022-03-22 | 江苏达胜高聚物股份有限公司 | High-thermal-conductivity silicone rubber cable material and preparation method and application thereof |
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