CN107267162A - A kind of preparation method of nano concave soil base inorganic flame-retarded agent - Google Patents

Abstract

The invention discloses a method for preparing a nano attapulgite-based inorganic flame retardant. The specific steps of the preparation method of the nano attapulgite-based inorganic flame retardant are as follows: S1: material selection of attapulgite, S2: stirring and mixing of attapulgite, S3 : mixing and adding of the first auxiliary material, S4: standing still, S5: filtration treatment, S6: secondary grinding treatment, S7: mixing and adding of the second auxiliary material. In the present invention, the use of attapulgite can obtain the viscosity of attapulgite, and at the same time, the flame retardancy of attapulgite can be effectively utilized, and the flame retardancy of attapulgite can be fully utilized, and at the same time, the addition of other first auxiliary materials and second auxiliary materials can further Improve the flame retardant performance, and at the same time can obtain good adhesive performance, more convenient to use.

Description

A kind of preparation method of nano-attapulgite-based inorganic flame retardant

technical field

The invention relates to the technical field of flame retardant improvement, in particular to a method for preparing a nano attapulgite-based inorganic flame retardant.

Background technique

Attapulgite is the abbreviation of Attapulgite Clay. It is a rare non-metallic mineral resource, it is a layer chain structure of water-rich magnesium aluminum silicate clay mineral.

As an important scarce non-metallic mineral resource, attapulgite has been widely used in more than 10 fields such as agriculture, animal husbandry, building materials, petroleum, metallurgy, and food. Attapulgite clay is one of the dominant non-metallic minerals in my country. It has a wide range of uses and is known as "the soil with thousands of uses and the king of all soils". The ice pack with attapulgite is still not frozen at minus 40 degrees, the steamed buns can be kept fresh for 8 months in a sealed jar made of attapulgite, and the handicrafts made of attapulgite can purify the air. Attapulgite has the functions of sterilization, deodorization, detoxification and insecticide. If it is used for diarrhea, it is used to absorb the poisonous bacteria in the stomach; the fine needle-shaped particles of the attapulgite will abrade the surface of the insects and adsorb the lipid compounds of the insects, resulting in the rapid death of the insects. It is also used in the military industry to absorb poisonous gas in protective devices and absorb animals. , vegetable oil pigment, aflatoxin and odor, etc. In the brewing industry, using attapulgite to clarify wine, cider, beer and other wine products can remove various residues and impurities in the wine and make the wine quality pure. From a chemical point of view, attapulgite has surface active centers, which not only adsorb, but also catalyze. Attapulgite can be used as a catalyst for the conversion of ethanol to ethylene, and also as a catalyst carrier. At the same time, the processed attapulgite clay products are ideal adsorbents, food processing aids and food additives, which can replace activated carbon. It is used in the ingredients of instant noodles that many people eat.

Using attapulgite as the matrix of flame retardant can take advantage of the flame retardancy of attapulgite, so that attapulgite can be effectively used. At the same time, the development of attapulgite as a matrix flame retardant is a problem we need to face.

Contents of the invention

The object of the present invention is to provide a kind of preparation method of nano attapulgite-based inorganic flame retardant, the specific steps of the preparation method of this nano attapulgite-based inorganic flame retardant are as follows:

S1: Material selection of attapulgite. Attapulgite with a purity higher than 98% is selected as the attapulgite base. The attapulgite is ground and sieved after grinding. The mesh of the attapulgite powder is 2000-3000 mesh. The attapulgite powder is placed for later use;

S2: Stirring and mixing of attapulgite, mixing attapulgite powder and water in a mixing ratio of 1:5 by weight and component, then mixing and stirring in a mixer, the speed of the mixer is 1200-1500 rpm, and the mixing time is controlled at 30-50 minutes;

S3: Mixing and adding of the first auxiliary material, after adding the auxiliary material, continue mixing and stirring for 10-15 minutes, the speed of the mixer is 600-800 rpm, and the mixing and stirring after the auxiliary material is added adopts heating type mixing and stirring, heating and mixing When the temperature is 80-95 ℃;

S4: Stand still, take out the material after heating and stirring and place it in a container for standing still, the standing time is at least 3-5 hours;

S5: Filtration treatment, filter and remove the supernatant of the solution after standing still, take out the bottom sediment, and dry it in the drying equipment. The drying temperature is controlled at 150-180 ° C, and the drying time is 30-40 minutes ;

S6: secondary grinding treatment, take out the dried material and carry out secondary grinding treatment in the grinding equipment, the powder mesh number after the secondary grinding treatment is 2000-2500 mesh, take out after grinding and set aside;

S7: Mix and add the second auxiliary material. After adding the second auxiliary material, mix, heat and stir. The heating temperature is 110-130°C. After mixing and stirring evenly, carry out cooling treatment. After cooling down to room temperature, carry out bagging and sealing for later use, and complete the nano attapulgite The processing of base inorganic flame retardants.

Preferably, the first auxiliary material is made of a flame retardant, a curing agent and a char-forming agent according to a ratio of 1:1:1 by weight, and the amount of the first auxiliary material is 15-18% of the total weight of attapulgite. %.

Preferably, the flame retardant is magnesium hydroxide, the curing agent methyl ethyl ketone peroxide and cobalt octanoate solution are prepared in a ratio of 2:1 by weight, and the char-forming agent is corn starch.

Preferably, the second auxiliary material is made of flame-retardant fiber and epoxy vinyl ester resin in a ratio of 1:5, and the amount of the second auxiliary material is 13-15% of the total weight of attapulgite.

Preferably, the flame-retardant fiber is decabromodiphenylethane flame-retardant high-strength vinylon, and the epoxy vinyl ester resin is flame-retardant epoxy vinyl ester resin.

Compared with the prior art, the beneficial effect of the present invention is: the use of the attapulgite in the present invention can obtain the viscosity of the attapulgite, and at the same time effectively utilize the flame retardancy of the attapulgite, and make full use of the flame retardancy of the attapulgite, At the same time, the addition of other first auxiliary materials and second auxiliary materials can further improve the flame retardant performance, and at the same time can obtain good adhesive performance and be more convenient to use.

detailed description

In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.

Example 1

A method for preparing a nano attapulgite-based inorganic flame retardant, the specific steps of the preparation method of the nano attapulgite-based inorganic flame retardant are as follows:

S1: Material selection of attapulgite. Attapulgite with a purity higher than 98% is selected as the attapulgite base. The attapulgite is ground and sieved after grinding. The mesh of the attapulgite powder is 2000-3000 mesh. The attapulgite powder is placed for later use;

S2: Stirring and mixing of attapulgite, mixing attapulgite powder and water according to the weight-to-component ratio of 1:5, and then mixing and stirring in the mixer. The speed of the mixer is 1200 rpm, and the mixing and stirring time is controlled at 30 minutes. ;

S3: The mixing and adding of the first auxiliary material, after adding the auxiliary material, continue mixing and stirring for 10 minutes, the speed of the mixer is 600 rpm, and the mixing and stirring after the auxiliary material is added adopts the heating type mixing and stirring, and the temperature during heating and mixing is at 80°C;

S4: Stand still, take out the heated and stirred material and place it in a container for standing still, the standing time is at least 3 hours;

S5: Filtration treatment, filter and remove the supernatant of the solution after standing still, take out the bottom sediment, and perform drying treatment in the drying equipment, the drying temperature is controlled at 150 ° C, and the drying time is 30 minutes;

S6: secondary grinding treatment, take out the dried material and carry out secondary grinding treatment in the grinding equipment, the powder mesh number after the secondary grinding treatment is 2000 mesh, take out after grinding and set aside;

S7: Mixing and adding of the second auxiliary material. After adding the second auxiliary material, mix and heat and stir. The heating temperature is 110°C. After mixing and stirring evenly, the temperature is lowered. After cooling to room temperature, it is bagged and sealed for later use. Processing of flame retardants.

The first auxiliary material is made of a flame retardant, a curing agent and a char forming agent according to a weight component ratio of 1:1:1, and the amount of the first auxiliary material is 15% of the total weight of the attapulgite. The flame retardant is magnesium hydroxide, the curing agent methyl ethyl ketone peroxide and cobalt octoate liquid are prepared according to the weight component ratio of 2:1, and the char forming agent is corn starch. The second auxiliary material is made of flame-retardant fiber and epoxy vinyl ester resin in a ratio of 1:5, and the amount of the second auxiliary material is 13% of the total weight of attapulgite. The flame-retardant fiber is decabromodiphenylethane flame-retardant high-strength vinylon, and the epoxy vinyl ester resin is flame-retardant epoxy vinyl ester resin.

Example 2

A method for preparing a nano attapulgite-based inorganic flame retardant, the specific steps of the preparation method of the nano attapulgite-based inorganic flame retardant are as follows:

S1: material selection of attapulgite, choose attapulgite with a purity higher than 98% as the attapulgite base, grind the attapulgite, and sieve the attapulgite powder after grinding. The powder is stored for later use;

S2: Stirring and mixing of attapulgite, mixing attapulgite powder and water according to the weight-to-component ratio of 1:5, and then mixing and stirring in the mixer. The speed of the mixer is 1400 rpm, and the mixing and stirring time is controlled at 40 minutes. ;

S3: The mixing and adding of the first auxiliary material, after adding the auxiliary material, continue mixing and stirring for 13 minutes, the speed of the mixer is 700 rpm, and the mixing and stirring after the auxiliary material is added adopts the heating type mixing and stirring, and the temperature during heating and mixing is at 85°C;

S4: Stand still, take out the heated and stirred material and place it in a container for standing still, the standing time is at least 4 hours;

S5: Filtration treatment, filter and remove the upper clear liquid of the solution after standing, take out the bottom sediment, and perform drying treatment in the drying equipment, the drying temperature is controlled at 170°C, and the drying time is 35 minutes;

S6: secondary grinding treatment, take out the dried material and carry out secondary grinding treatment in the grinding equipment, the powder mesh number after the secondary grinding treatment is 2300 mesh, take out after grinding and set aside;

S7: Mixing and adding of the second auxiliary material. After adding the second auxiliary material, mix and heat and stir. The heating temperature is 120°C. After mixing and stirring evenly, the temperature is lowered. Processing of flame retardants.

The first auxiliary material is made of a flame retardant, a curing agent and a char-forming agent according to a weight component ratio of 1:1:1, and the amount of the first auxiliary material is 16% of the total weight of attapulgite. The flame retardant is magnesium hydroxide, the curing agent methyl ethyl ketone peroxide and cobalt octoate liquid are prepared according to the weight component ratio of 2:1, and the char forming agent is corn starch. The second auxiliary material is made of flame-retardant fiber and epoxy vinyl ester resin in a ratio of 1:5, and the amount of the second auxiliary material is 14% of the total weight of attapulgite. The flame-retardant fiber is decabromodiphenylethane flame-retardant high-strength vinylon, and the epoxy vinyl ester resin is flame-retardant epoxy vinyl ester resin.

Example 3

A method for preparing a nano attapulgite-based inorganic flame retardant, the specific steps of the preparation method of the nano attapulgite-based inorganic flame retardant are as follows:

S1: material selection of attapulgite, choose attapulgite with a purity higher than 98% as the attapulgite base, grind the attapulgite, and then sieve the attapulgite powder after grinding. The powder is stored for later use;

S2: Stirring and mixing of attapulgite, mixing attapulgite powder and water according to the weight-to-component ratio of 1:5, and then mixing and stirring in the mixer. The speed of the mixer is 1500 rpm, and the mixing and stirring time is controlled at 50 minutes. ;

S3: The mixing and adding of the first auxiliary material, after adding the auxiliary material, continue mixing and stirring for 15 minutes, the speed of the mixer is 800 rpm, and the mixing and stirring after the auxiliary material is added adopts the heating type mixing and stirring, and the temperature during heating and mixing is at 95°C;

S4: Stand still, take out the heated and stirred material and place it in a container for standing still, the standing time is at least 5 hours;

S5: Filtration treatment, filter and remove the upper clear liquid of the solution after standing still, take out the bottom sediment, and perform drying treatment in the drying equipment, the drying temperature is controlled at 180 ° C, and the drying time is 40 minutes;

S6: secondary grinding treatment, take out the dried material and carry out secondary grinding treatment in the grinding equipment, the powder mesh number after the secondary grinding treatment is 2500 mesh, take out after grinding and set aside;

S7: The second auxiliary material is mixed and added. After adding the second auxiliary material, mix, heat and stir. The heating temperature is 130°C. After mixing and stirring evenly, the temperature is lowered. After cooling to room temperature, it is bagged and sealed for later use. Processing of flame retardants.

The first auxiliary material is made of a flame retardant, a curing agent and a char-forming agent according to a weight component ratio of 1:1:1, and the amount of the first auxiliary material is 18% of the total weight of attapulgite. The flame retardant is magnesium hydroxide, the curing agent methyl ethyl ketone peroxide and cobalt octoate liquid are prepared according to the weight component ratio of 2:1, and the char forming agent is corn starch. The second auxiliary material is made of flame-retardant fiber and epoxy vinyl ester resin in a ratio of 1:5, and the amount of the second auxiliary material is 15% of the total weight of attapulgite. The flame-retardant fiber is decabromodiphenylethane flame-retardant high-strength vinylon, and the epoxy vinyl ester resin is flame-retardant epoxy vinyl ester resin.

In the present invention, the use of attapulgite can obtain the viscosity of attapulgite, and at the same time, the flame retardancy of attapulgite can be effectively utilized, and the flame retardancy of attapulgite can be fully utilized, and at the same time, the addition of other first auxiliary materials and second auxiliary materials can further improve Improve the flame retardant performance, and at the same time can obtain good adhesive performance, more convenient to use.

The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto, any person familiar with the technical field within the technical scope disclosed in the present invention, according to the technical solution of the present invention Any equivalent replacement or change of the inventive concepts thereof shall fall within the protection scope of the present invention.

Claims (5)

1. A preparation method for a nano-attapulgite-based inorganic flame retardant, characterized in that: the specific steps of the preparation method of the nano-attapulgite-based inorganic flame retardant are as follows: S1: Material selection of attapulgite. Attapulgite with a purity higher than 98% is selected as the attapulgite base. The attapulgite is ground and sieved after grinding. The mesh of the attapulgite powder is 2000-3000 mesh. The attapulgite powder is placed for later use; S2: Stirring and mixing of attapulgite, mixing attapulgite powder and water according to the weight-to-component ratio of 1:5, and then mixing and stirring in the mixer. The speed of the mixer is 1200-1500 rpm, and the mixing time is controlled at 30-50 minutes; S3: Mixing and adding of the first auxiliary material, after adding the auxiliary material, continue mixing and stirring for 10-15 minutes, the speed of the mixer is 600-800 rpm, and the mixing and stirring after the auxiliary material is added adopts heating type mixing and stirring, heating and mixing When the temperature is 80-95 ℃; S4: Stand still, take out the material after heating and stirring and place it in a container for standing still, the standing time is at least 3-5 hours; S5: Filtration treatment, filter and remove the supernatant of the solution after standing still, take out the bottom sediment, and dry it in the drying equipment. The drying temperature is controlled at 150-180 ° C, and the drying time is 30-40 minutes ; S6: secondary grinding treatment, take out the dried material and carry out secondary grinding treatment in the grinding equipment, the powder mesh number after the secondary grinding treatment is 2000-2500 mesh, take out after grinding and set aside; S7: Mix and add the second auxiliary material. After adding the second auxiliary material, mix, heat and stir. The heating temperature is 110-130°C. After mixing and stirring evenly, carry out cooling treatment. After cooling down to room temperature, carry out bagging and sealing for later use, and complete the nano attapulgite The processing of base inorganic flame retardants. 2. The preparation method of a kind of nano-attapulgite-based inorganic flame retardant according to claim 1, characterized in that: the first auxiliary material is a flame retardant, a curing agent and a char-forming agent according to a weight-to-component ratio of 1 : 1:1 ratio, the amount of the first auxiliary material is 15-18% of the total weight of attapulgite. 3. the preparation method of a kind of nano attapulgite-based inorganic flame retardant according to claim 2, is characterized in that: described flame retardant is magnesium hydroxide, and described curing agent methyl ethyl ketone peroxide and cobalt octanoate liquid are by weight The component ratio is 2:1, and the char-forming agent is corn starch. 4. The preparation method of a kind of nano-attapulgite-based inorganic flame retardant according to claim 1, characterized in that: the second auxiliary material is made of flame-retardant fiber and epoxy vinyl ester resin according to the ratio of 1:5 into, and the amount of the second auxiliary material is 13-15% of the total weight of attapulgite. 5. The preparation method of a kind of nano-attapulgite-based inorganic flame retardant according to claim 4, characterized in that: the flame-retardant fiber is decabromodiphenylethane flame-retardant high-strength vinylon, and the epoxy vinyl The ester resin is a flame retardant epoxy vinyl ester resin.