CN112321900A - Bentonite for flame retardant and preparation method thereof - Google Patents
Bentonite for flame retardant and preparation method thereof Download PDFInfo
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- CN112321900A CN112321900A CN202011319990.7A CN202011319990A CN112321900A CN 112321900 A CN112321900 A CN 112321900A CN 202011319990 A CN202011319990 A CN 202011319990A CN 112321900 A CN112321900 A CN 112321900A
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- bentonite
- flame retardant
- slurry
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- dispersant
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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
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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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K5/00—Use of organic ingredients
- C08K5/02—Halogenated hydrocarbons
-
- 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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
- C08K5/523—Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- 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
Abstract
The invention discloses a preparation method of bentonite for a flame retardant, which comprises the following steps: (1) adding water into bentonite to prepare high-concentration slurry with the concentration of 3-20%; (2) heating the bentonite slurry to 40-80 ℃, and preserving heat for 24-48 hours; (3) adding water into the bentonite slurry for dispersion, and adding a dispersant; (4) heating to 40-80 deg.C, and stirring at high speed of 100-2000 rpm for 30-240 min; (5) dehydrating, drying and crushing to obtain the bentonite for the flame retardant. The bentonite of the invention keeps the special layered structure and dispersion form of the bentonite to the maximum extent, has the function of blocking heat and combustible gas generated during combustion, is easy to migrate and enrich in a matrix material, can effectively catalyze to form carbon, further strengthens the blocking function of the system by the carbon layer, and improves the flame retardance of the composite flame retardant material.
Description
Technical Field
The invention belongs to the field of high polymer flame retardants, relates to a flame retardant component, and more particularly relates to bentonite for a flame retardant.
Background
The high polymer has the characteristic of being very easy to burn, and is very easy to cause fire. The oxygen index of the high polymers is mostly less than 20%. The combustion process produces a large amount of smoke and releases a lot of heat and toxic gases. Causing great loss to national economy, personal safety, environment and the like. Therefore, the flame retardant research of high polymers becomes one of the important research hotspots of the polymer material science, and receives high attention at home and abroad.
The bentonite is a clay material with a lamellar structure, and has good application potential in the field of flame retardance. Related research is also done by researchers in China. For example, a composite flame retardant containing modified nano-bentonite (No. CN 103788678B), discloses a composite flame retardant containing modified nano-bentonite, is prepared by adding the modified nano-bentonite into the flame retardant and adjusting the formula, has the advantages of low price, low smoke, small usage amount, good flame retardant effect, no toxicity, no pollution and the like, and is a composite flame retardant with good smoke suppression performance, good flame retardant performance, environmental protection and the like. A low toxicity flame retardant (application No. 201611108755.9) is provided. The components include bentonite, dicyclo hypophosphite, magnesium hydroxide, sodium bicarbonate, etc.
However, these studies do not relate to the morphology of the lamellar structure of bentonite and the effect of the lamellar structure on the flame retardancy and the physical properties of the polymer.
Disclosure of Invention
The invention aims to provide bentonite applied to the field of high polymer flame retardance and a preparation method thereof. The invention utilizes high-concentration, high-temperature and high-speed hydraulic stripping process to replace powder grinding process, so as to obtain the bentonite which is fully stripped and keeps complete lamellar structure.
The preparation method of the bentonite for the flame retardant is characterized by comprising the following steps:
(1) adding water into bentonite to prepare high-concentration slurry with the concentration of 3-20%;
(2) heating the bentonite slurry to 40-80 ℃, and preserving heat for at least 1 hour;
(3) dispersing the bentonite slurry in water, and adding a dispersant, wherein the addition amount of the dispersant is 0.1-1.0% of the amount of the bentonite; the concentration of the dispersed slurry is 1-5%;
(4) heating the bentonite slurry prepared in the step (3) to 40-80 ℃, and then stirring at a high speed at a rotating speed of 100-2000 rpm for 30-240 minutes;
(5) and (4) dehydrating, drying and crushing the bentonite slurry prepared in the step (4) to obtain the bentonite for the flame retardant.
Further, the high-concentration slurry in the step (1) has the concentration of 5-10%.
Further, the temperature in the step (2) is 60-80 ℃.
Further, in the step (3), the dispersant is sodium hexametaphosphate, sodium pyrophosphate, phosphate ester or high polymer dispersant.
Further, in the step (4), the temperature is 60-80 ℃, the stirring speed is 1500-2000 r/min, and the stirring time is 60-180 min.
The invention also provides bentonite for the flame retardant, which is prepared by the preparation method.
The invention also provides a high polymer flame retardant, which comprises the bentonite for the flame retardant prepared by the method.
The bentonite of the invention keeps the special layered structure and dispersion form of the bentonite to the maximum extent, has the function of blocking heat and combustible gas generated during combustion, is easy to migrate and enrich in a matrix material, can effectively catalyze to form carbon, further strengthens the blocking function of the system by the carbon layer, and improves the flame retardance of the composite flame retardant material.
The surface of the bentonite has active points with large activity, has unpaired electrons and can play a chemical role with high polymers. The polymer chains are adsorbed on the surface of the bentonite, and a plurality of points are chemically combined with the surface of the bentonite, so that the effect is called chemical adsorption, and the chemical adsorption is much larger than the simple physical adsorption. The chemical adsorption is characterized in that molecular chains are easier to move on the surface of the bentonite, but are not easy to separate from the bentonite. Thus, the high polymer and the bentonite form a strong bond capable of sliding, and the strength of the high polymer is increased.
The excellent barrier property of the bentonite enables the bentonite to gradually migrate to the surface of the material during combustion, the stability and the barrier property of the expanded carbon layer are improved, and the smoke release rate of the material is further reduced.
The bentonite for the flame retardant is compounded with the existing flame retardant for application, so that the flame retardant property of the high polymer can be obviously improved, and the physical property of the high polymer can be improved.
Detailed Description
Example 1
Example 1
100g of bentonite is taken and added with water to prepare high-concentration slurry with the concentration of 10 percent, the temperature is heated to 60 ℃, and the heat preservation is carried out for 24 hours. Then, water and 0.5g of a dispersant sodium hexametaphosphate were added, dispersed to a concentration of 4%, and heated to 80 ℃ and stirred at high speed for 60 minutes at a stirring speed of 1500 rpm. And after the reaction is finished, dehydrating, drying and crushing to obtain a finished product.
The prepared modified bentonite and halogen flame retardant chlorinated alicyclic hydrocarbon are uniformly added into ABS plastic.
The ABS plastic properties were tested as follows:
the results show that the oxygen index and GWIT of the flame retardant property index are improved after the modified bentonite is added; the strength index of the plastic is improved.
Example 2
1 ton of bentonite is added with water to prepare high-concentration slurry with the concentration of 8 percent, the temperature is heated to 70 ℃, and the temperature is kept for 48 hours. Then, water and 40kg of a phosphate ester dispersant were added, dispersed to a concentration of 5%, and heated to 70 ℃ and stirred at a high speed of 2000 rpm for 120 minutes. And after the reaction is finished, dehydrating, drying and crushing to obtain a finished product.
The prepared modified bentonite and phosphorus flame retardant ditolyl phosphate are uniformly added into PP plastic.
The PP plastic properties were tested as follows:
the results show that the oxygen index and GWIT of the flame retardant property index are improved after the modified bentonite is added; the strength index of the plastic is improved.
Example 3
1 ton of bentonite is added with water to prepare high-concentration slurry with the concentration of 5 percent, the temperature is heated to 80 ℃, and the temperature is kept for 36 hours. Then, water and 60 phosphate ester dispersant were added, dispersed to a concentration of 3%, and heated to 80 ℃ and stirred at high speed for 180 minutes at a stirring speed of 1500 rpm. And after the reaction is finished, dehydrating, drying and crushing to obtain a finished product.
The prepared modified bentonite, antimony flame retardant (antimony trioxide + tetrachlorophthalic anhydride) and halogen flame retardant are uniformly added into PE plastic.
The PE plastic properties were tested as follows:
the results show that the oxygen index and GWIT of the flame retardant property index are improved after the modified bentonite is added; the strength index of the plastic is improved.
It can be seen from the above examples that the bentonite for flame retardant of the invention, when used in combination with the existing flame retardant, can significantly improve the flame retardant property of the high polymer and can improve the physical properties of the high polymer.
Finally, the foregoing disclosure is directed to only certain embodiments of the invention. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (7)
1. The preparation method of the bentonite for the flame retardant is characterized by comprising the following steps:
(1) adding water into bentonite to prepare high-concentration slurry with the concentration of 3-20%;
(2) heating the bentonite slurry to 40-80 ℃, and preserving heat for 24-48 hours;
(3) dispersing the bentonite slurry in water, and adding a dispersant, wherein the addition amount of the dispersant is 0.1-1.0% of the amount of the bentonite; the concentration of the dispersed bentonite slurry is 1-5%;
(4) heating the bentonite slurry prepared in the step (3) to 40-80 ℃, and then stirring at a high speed at a rotating speed of 100-2000 rpm for 30-240 minutes;
(5) and (4) dehydrating, drying and crushing the bentonite slurry prepared in the step (4) to obtain the bentonite for the flame retardant.
2. The method according to claim 1, wherein the high consistency slurry in the step (1) has a consistency of 5 to 10%.
3. The method according to claim 1, wherein the temperature in the step (2) is 60 to 80 ℃.
4. The method according to claim 1, wherein the dispersant in the step (3) is sodium hexametaphosphate, sodium pyrophosphate, phosphate ester or a high polymer dispersant.
5. The process according to claim 1, wherein the temperature in the step (4) is 60 to 80 ℃, the stirring speed is 1500 to 2000 rpm, and the stirring time is 60 to 180 minutes.
6. The bentonite for flame retardant, which is produced by the production method according to any one of claims 1 to 5.
7. A high polymer flame retardant, characterized in that the high polymer flame retardant comprises the bentonite for flame retardant prepared by the preparation method of any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011319990.7A CN112321900A (en) | 2020-11-23 | 2020-11-23 | Bentonite for flame retardant and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011319990.7A CN112321900A (en) | 2020-11-23 | 2020-11-23 | Bentonite for flame retardant and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN112321900A true CN112321900A (en) | 2021-02-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011319990.7A Pending CN112321900A (en) | 2020-11-23 | 2020-11-23 | Bentonite for flame retardant and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5391228A (en) * | 1990-12-21 | 1995-02-21 | Southern Clay Products, Inc. | Method for preparing high solids bentonite slurries |
| JP2005015692A (en) * | 2003-06-27 | 2005-01-20 | Daicel Polymer Ltd | Flame retardant resin composition |
| CN102604441A (en) * | 2012-03-21 | 2012-07-25 | 山东理工大学 | Organic bentonite for composite flame retardants and preparation process thereof |
| CN104130562A (en) * | 2014-07-28 | 2014-11-05 | 江苏嘉铂新材料有限公司 | Nano-bentonite composite flame-retardant polyhydroxybutyrate bioplastic and preparation method thereof |
| CN110357118A (en) * | 2019-08-29 | 2019-10-22 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of bentonite prepares the low energy consumption production technology of inorganic gel |
-
2020
- 2020-11-23 CN CN202011319990.7A patent/CN112321900A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5391228A (en) * | 1990-12-21 | 1995-02-21 | Southern Clay Products, Inc. | Method for preparing high solids bentonite slurries |
| JP2005015692A (en) * | 2003-06-27 | 2005-01-20 | Daicel Polymer Ltd | Flame retardant resin composition |
| CN102604441A (en) * | 2012-03-21 | 2012-07-25 | 山东理工大学 | Organic bentonite for composite flame retardants and preparation process thereof |
| CN104130562A (en) * | 2014-07-28 | 2014-11-05 | 江苏嘉铂新材料有限公司 | Nano-bentonite composite flame-retardant polyhydroxybutyrate bioplastic and preparation method thereof |
| CN110357118A (en) * | 2019-08-29 | 2019-10-22 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of bentonite prepares the low energy consumption production technology of inorganic gel |
Non-Patent Citations (1)
| Title |
|---|
| 李鑫: "低品质膨润土提质改性技术研究", 《硅酸盐通报》 * |
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Application publication date: 20210205 |