CN110564006A - Flame retardant for low-density polyethylene, preparation method and application thereof - Google Patents
Flame retardant for low-density polyethylene, preparation method and application thereof Download PDFInfo
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- CN110564006A CN110564006A CN201910860969.9A CN201910860969A CN110564006A CN 110564006 A CN110564006 A CN 110564006A CN 201910860969 A CN201910860969 A CN 201910860969A CN 110564006 A CN110564006 A CN 110564006A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K3/2279—Oxides; Hydroxides of metals of antimony
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/02—Halogenated hydrocarbons
- C08K5/03—Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
Abstract
The invention discloses a flame retardant for low-density polyethylene, a preparation method and application thereof, and belongs to the technical field of composite flame retardants. The flame retardant comprises the following raw materials in parts by weight: 4-21 parts of antimony trioxide, 13-63 parts of decabromodiphenylethane and 17-83 parts of modified magnesium hydroxide; the flame retardant is prepared by uniformly mixing antimony trioxide, decabromodiphenylethane and modified magnesium hydroxide in parts by weight. The invention integrates the advantages of halogen flame retardant and inorganic flame retardant, solves the problems of serious dripping and large smoke generation amount during the combustion of the low-density polyethylene under the condition of ensuring the tensile strength, hardness, bending strength and impact strength of the low-density polyethylene base material, improves the limit oxygen index of the composite flame retardant material, and reduces the using amounts of antimony trioxide and decabromodiphenylethane.
Description
Technical Field
The invention belongs to the technical field of composite flame retardants, and particularly relates to a flame retardant for low-density polyethylene, a preparation method and application thereof.
Background
Polyethylene is the variety with the largest capacity and the largest import in Chinese synthetic resin. Polyethylene is mainly classified into linear low density polyethylene, low density polyethylene and high density polyethylene. The composite material is mainly applied to various injection molding and blow molding products, pipe materials, electric wire and cable insulation and sheaths, and the like. The polyethylene has excellent physical and mechanical properties, electrical properties and chemical corrosion resistance, and particularly has good processing performance, so the polyethylene has extremely wide application. Because the polyethylene is extremely easy to burn, the oxygen index of the polyethylene is only 17 percent, the polyethylene has serious melting and dropping during burning, large smoke amount and potential fire risk in the using process, and the polyethylene is very necessary to be subjected to flame retardant modification.
Chinese patent application document 'an intumescent flame retardant for flame-retardant low-density polyethylene (patent application number: 201810057187.7)' discloses a flame retardant, which is prepared by melt blending of modified red mud, ammonium polyphosphate, pentaerythritol, melamine and low-density polyethylene, wherein the oxygen index of the prepared low-density polyethylene composite material reaches over 29.0%, and the vertical combustion grade reaches UL94 and V-0 grades.
Chinese patent application document 'a composite flame retardant for low-density polyethylene (patent application No. 201810111891.6)' discloses a flame retardant, which consists of antimony trioxide, decabromodiphenylethane and phthalate ester coupling agent NDZ-201 modified bentonite.
the modified magnesium hydroxide replaces part of the halogen antimony flame retardant, and the advantages of the inorganic flame retardant and the halogen flame retardant can be combined, so that the using amount of the halogen flame retardant is reduced, and the adding amount of the flame retardant is reduced. The problems of serious melting and dropping and large smoke generation amount of the low-density polyethylene during combustion are solved under the condition of ensuring the mechanical property of the low-density polyethylene, the limit oxygen index of the composite flame-retardant material is improved, and the cost is reduced.
The above background disclosure is only for the purpose of assisting understanding of the concept and technical solution of the present invention and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed at the filing date of the present patent application.
Disclosure of Invention
The invention provides a flame retardant for low-density polyethylene, a preparation method and application thereof, aiming at solving the practical problems of how to improve the limiting oxygen index and reduce the cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
A flame retardant for low-density polyethylene comprises the following raw materials in parts by weight: 4-21 parts of antimony trioxide, 13-63 parts of decabromodiphenylethane and 17-83 parts of modified magnesium hydroxide.
Preferably, the flame retardant for low-density polyethylene comprises the following raw materials in parts by weight: 17 parts of antimony trioxide, 50 parts of decabromodiphenylethane and 33 parts of modified magnesium hydroxide.
Preferably, the mass ratio of the antimony trioxide to the modified magnesium hydroxide is 1: 0.8 to 20.
Preferably, the preparation method of the modified magnesium hydroxide comprises the following steps: dissolving magnesium hydroxide in distilled water, controlling the temperature within the range of 30-90 ℃, uniformly stirring and dispersing, adding pentaerythritol stearate into absolute ethyl alcohol, dissolving at the temperature of 50-90 ℃, adding the dissolved pentaerythritol stearate solution into the magnesium hydroxide solution, stirring at constant temperature for 1-60 min, filtering after the reaction is finished, putting the mixture into an oven, drying at the temperature of 90 ℃, cooling, and sieving with a 200-mesh sieve to obtain the modified magnesium hydroxide.
Preferably, the weight part of magnesium hydroxide dissolved in distilled water is 100 parts.
Preferably, the liquid-solid ratio of the distilled water to the magnesium hydroxide is 15-30.
Preferably, the pentaerythritol stearate is added to the absolute ethyl alcohol in a weight part of 0.4 to 1.6 parts.
The invention also provides a preparation method of the flame retardant for low-density polyethylene, which is prepared by uniformly mixing antimony trioxide, decabromodiphenylethane and modified magnesium hydroxide in parts by weight.
the invention also provides an application of the flame retardant for the low-density polyethylene, which is applied to the preparation of the low-density polyethylene and comprises 6-24% of the flame retardant for the low-density polyethylene by mass fraction.
Preferably, the method is applied to preparing low-density polyethylene, and the low-density polyethylene comprises 18% of flame retardant for the low-density polyethylene by mass fraction.
Compared with the prior art, the invention has the beneficial effects that:
(1) The single antimony halide flame retardant used for polyethylene production has the problems of high price, large smoke generation amount, serious melting and dripping and the like. And the carbonization of the material can be promoted to form a carbon layer, so that the problems of material melt dripping and large combustion smoke generation after the halogen antimony flame retardant is added are effectively inhibited. The limited oxygen index of the material can be improved to 34.9% by adding a certain amount of the composite flame retardant, so that the synergistic flame retardant performance of the modified magnesium hydroxide and the halogen antimony flame retardant has great feasibility. The invention can not only reduce the dosage of the halogen antimony flame retardant, but also effectively reduce the cost of the flame retardant.
(2) the modified magnesium hydroxide is used as one of the main components of the flame retardant, and can be better dispersed in a base material compared with unmodified magnesium hydroxide, so that the flame retardant effect of the composite flame retardant is enhanced; on the other hand, the problem that the inorganic flame retardant reduces the mechanical property of the base material can be avoided by the organically modified magnesium hydroxide, so that the composite flame-retardant material can meet more product requirements.
(3) The invention integrates the advantages of halogen flame retardant and inorganic flame retardant, does not generate melting and dripping in the combustion process, and has high char yield and stable char layer.
Detailed Description
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
Example 1
A flame retardant for low-density polyethylene comprises the following raw materials in parts by weight: 21 parts of antimony trioxide, 63 parts of decabromodiphenylethane and 17 parts of modified magnesium hydroxide.
The preparation method of the modified magnesium hydroxide comprises the following steps: adding 100 parts by weight of magnesium hydroxide into distilled water, controlling the liquid-solid ratio to be 15, uniformly stirring and dispersing under the condition of 30 ℃, adding 0.4 part of pentaerythritol stearate into absolute ethyl alcohol, dissolving at the temperature of 50-90 ℃, adding the dissolved pentaerythritol stearate solution into the magnesium hydroxide solution, stirring at constant temperature for 60min, filtering after the reaction is finished, drying in an oven at the temperature of 90 ℃, cooling, and sieving with a 200-mesh sieve to obtain the modified magnesium hydroxide.
The flame retardant of the low-density polyethylene is prepared by uniformly mixing antimony trioxide, decabromodiphenylethane and modified magnesium hydroxide according to parts by weight.
Example 2
A flame retardant for low-density polyethylene comprises the following raw materials in parts by weight: 17 parts of antimony trioxide, 50 parts of decabromodiphenylethane and 33 parts of modified magnesium hydroxide.
The preparation method of the modified magnesium hydroxide comprises the following steps: adding 100 parts by weight of magnesium hydroxide into distilled water, controlling the liquid-solid ratio to be 20, uniformly stirring and dispersing under the condition of 50 ℃, adding 0.8 part of pentaerythritol stearate into absolute ethyl alcohol, dissolving at the temperature of 50-90 ℃, adding the dissolved pentaerythritol stearate solution into the magnesium hydroxide solution, stirring at constant temperature for 45min, filtering after the reaction is finished, drying in an oven at the temperature of 90 ℃, cooling, and sieving with a 200-mesh sieve to obtain the modified magnesium hydroxide.
The flame retardant of the low-density polyethylene is prepared by uniformly mixing antimony trioxide, decabromodiphenylethane and modified magnesium hydroxide according to parts by weight.
Example 3
A flame retardant for low-density polyethylene comprises the following raw materials in parts by weight: 13 parts of antimony trioxide, 37 parts of decabromodiphenylethane and 50 parts of modified magnesium hydroxide.
The preparation method of the modified magnesium hydroxide comprises the following steps: adding 100 parts by weight of magnesium hydroxide into distilled water, controlling the liquid-solid ratio to be 25, uniformly stirring and dispersing under the condition of 70 ℃, adding 1.2 parts by weight of pentaerythritol stearate into absolute ethyl alcohol, dissolving at the temperature of 50-90 ℃, adding the dissolved pentaerythritol stearate solution into the magnesium hydroxide solution, stirring at constant temperature for 30min, filtering after the reaction is finished, drying in an oven at the temperature of 90 ℃, cooling, and sieving with a 200-mesh sieve to obtain the modified magnesium hydroxide.
The flame retardant of the low-density polyethylene is prepared by uniformly mixing antimony trioxide, decabromodiphenylethane and modified magnesium hydroxide according to parts by weight.
Example 4
A flame retardant for low-density polyethylene comprises the following raw materials in parts by weight: 4 parts of antimony trioxide, 13 parts of decabromodiphenylethane and 83 parts of modified magnesium hydroxide.
The preparation method of the modified magnesium hydroxide comprises the following steps: adding 100 parts by weight of magnesium hydroxide into distilled water, controlling the liquid-solid ratio to be 30, uniformly stirring and dispersing under the condition of 90 ℃, adding 1.6 parts by weight of pentaerythritol stearate into absolute ethyl alcohol, dissolving at the temperature of 50-90 ℃, adding the dissolved pentaerythritol stearate solution into the magnesium hydroxide solution, stirring at constant temperature for 15min, filtering after the reaction is finished, drying in an oven at the temperature of 90 ℃, cooling, and sieving with a 200-mesh sieve to obtain the modified magnesium hydroxide.
The flame retardant of the low-density polyethylene is prepared by uniformly mixing antimony trioxide, decabromodiphenylethane and modified magnesium hydroxide according to parts by weight.
Example 5
A low density polyethylene comprising a mass fraction of 24% of the flame retardant prepared in example 1.
Example 6
A low density polyethylene comprising a mass fraction of 24% of the flame retardant prepared in example 2.
Example 7
A low density polyethylene comprising a mass fraction of 24% of the flame retardant prepared in example 3.
Example 8
A low density polyethylene comprising 18% by weight of the flame retardant prepared in example 2.
Example 9
A low density polyethylene comprising 12% by weight of the flame retardant prepared in example 2.
Comparative example 1
A pure low density polyethylene comprising no flame retardant.
Comparative example 2
Chinese patent application document "A composite flame retardant for Low Density polyethylene (patent application No.: 201810111891.6)" the low Density polyethylene prepared in example 5.
Comparative example 3
The low density polyethylene prepared in example 6 of the chinese patent application "a composite flame retardant for low density polyethylene (patent application No.: 201810111891.6)".
Comparative example 4
Chinese patent application document "A composite flame retardant for Low Density polyethylene (patent application No.: 201810111891.6)" the low Density polyethylene prepared in example 7.
The specifically designed test method comprises the following steps:
The examples 5 to 9 and the comparative examples 1 to 4 were subjected to performance tests, and the performance such as the limiting oxygen index, the combustion grade, the bending strength and the tensile strength were mainly tested, and the test standards were GB/T2048-2008, GB/T1040-92 and GB/T9341-2000, respectively. The results of the various performance tests are shown in Table 1.
TABLE 1
From the experimental data of examples 5 to 9 and comparative examples 1 to 4, it is clear that the mechanical properties of the composite flame retardant of the present invention are not reduced while the flame retardancy of the material is greatly improved. The invention has the advantages of good flame retardant effect, low preparation cost and the like. Compared with the prior art, the limiting oxygen index of the invention is improved by at least 13.82%, therefore, the invention has outstanding progress and remarkable effect.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the preferred embodiments of the present invention are described in the above embodiments and the description only, and that the present invention is not limited thereto, and that various changes and modifications may be made without departing from the spirit and scope of the present invention, which fall within the scope of the claimed invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The flame retardant for the low-density polyethylene is characterized by comprising the following raw materials in parts by weight: 4-21 parts of antimony trioxide, 13-63 parts of decabromodiphenylethane and 17-83 parts of modified magnesium hydroxide.
2. The flame retardant for low-density polyethylene according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 17 parts of antimony trioxide, 50 parts of decabromodiphenylethane and 33 parts of modified magnesium hydroxide.
3. The flame retardant for low density polyethylene according to claim 1, characterized in that the mass ratio of antimony trioxide to modified magnesium hydroxide is 1: 0.8 to 20.
4. The flame retardant for low density polyethylene according to any one of claims 1 to 3, wherein the modified magnesium hydroxide is prepared by the following method: dissolving magnesium hydroxide in distilled water, controlling the temperature within the range of 30-90 ℃, uniformly stirring and dispersing, adding pentaerythritol stearate into absolute ethyl alcohol, dissolving at the temperature of 50-90 ℃, adding the dissolved pentaerythritol stearate solution into the magnesium hydroxide solution, stirring at constant temperature for 1-60 min, filtering after the reaction is finished, putting the mixture into an oven, drying at the temperature of 90 ℃, cooling, and sieving with a 200-mesh sieve to obtain the modified magnesium hydroxide.
5. The flame retardant for low density polyethylene according to claim 4, wherein the weight part of magnesium hydroxide dissolved in distilled water is 100 parts.
6. The flame retardant for low-density polyethylene according to claim 5, wherein the liquid-solid ratio of distilled water to magnesium hydroxide is 15 to 30.
7. The flame retardant for low density polyethylene according to claim 4, wherein the pentaerythritol stearate is added to the absolute ethyl alcohol in an amount of 0.4 to 1.6 parts by weight.
8. A preparation method of the flame retardant for the low-density polyethylene according to any one of claims 1 to 7, characterized in that the flame retardant is prepared by uniformly mixing antimony trioxide, decabromodiphenylethane and modified magnesium hydroxide according to parts by weight.
9. Use of a flame retardant according to any of claims 1-8 for low density polyethylene, characterized in that: the flame retardant is applied to preparation of low-density polyethylene and comprises 6-24% of flame retardant for the low-density polyethylene in mass fraction.
10. Use of a flame retardant according to claim 9 for low density polyethylene, characterized in that: the flame retardant is applied to preparing low-density polyethylene and comprises 18 mass percent of flame retardant for the low-density polyethylene.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910860969.9A CN110564006A (en) | 2019-09-11 | 2019-09-11 | Flame retardant for low-density polyethylene, preparation method and application thereof |
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| CN201910860969.9A CN110564006A (en) | 2019-09-11 | 2019-09-11 | Flame retardant for low-density polyethylene, preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113637253A (en) * | 2021-09-06 | 2021-11-12 | 江苏晶华新材料科技有限公司 | Preparation process of flame-retardant low-density polyethylene |
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| CN113637253A (en) * | 2021-09-06 | 2021-11-12 | 江苏晶华新材料科技有限公司 | Preparation process of flame-retardant low-density polyethylene |
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Application publication date: 20191213 |