CN1824730A - Manufacture of ultra fine red phosphorus composite fire retardant and its product using air bubble liquid film method - Google Patents
Manufacture of ultra fine red phosphorus composite fire retardant and its product using air bubble liquid film method Download PDFInfo
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Abstract
The present invention relates to a bubble liquid film method for preparing ultramicro red phosphorus composite fire retarding agent and its product. It is characterized by that said method includes the following steps: adopting bubble liquid film reactor, using one, two or more than two aqueous solutions of water-soluble salts, oxides or hydroxides of magnesium, aluminium, calcium, zinc and silicon elements as raw material, using one, two or more than two aqueous solutions or gases of NaOH, NH3-H2O, NH3 and Ca(OH)2 as settling agent, making the red phosphorus be dispersed in raw material aqueous solution or settling agent aqueous solution to form ultramicro red phosphorus particles, using one, two or more than two fatty acids (salts) and polyunsaturated fatty acids (salts) as surface modifying agent, in the bubble liquid film reactor utilizing bubbles to partition reaction liquid into liquid film, making reactant be reacted in liquid film to form ultramicro particles of correspondent hydroxide, oxide or salt to cover the ultramicro red phosphorus particles in the liquid film so as to obtain the invented ultramicro red phosphorus composite fire retarding agent.
Description
[ technical field]A method for producing a semiconductor device
The invention relates to a method for preparing an ultramicro red phosphorus composite flame retardant and a product by a bubble liquid film method, belonging to the manufacturing industry of inorganic chemical nano materials.
[ background of the invention]
Due to the strict requirements of environmental protection, halogen-free flame retardants are urgently needed for flame-retardant polymer materials. The flame retardants such as red phosphorus/magnesium hydroxide, red phosphorus/aluminum hydroxide and the like can meet the market requirements of halogen-free flame retardants.
The red phosphorus and organic matters produce violent dehydration and carbon formation when being combusted, can effectively prevent combustion, has good flame retardant effect, and can be widely used as a flame retardant for high polymer materials such as rubber, plastics and the like. It is used in large quantities in the last 80 years abroad. The red phosphorus flame-retardant material is researched from90 years. The colloidal red phosphorus, the microcapsule red phosphorus and the red phosphorus master batch are developed in sequence, and new products are listed in succession. However, due to the problem of accurate weighing of colloidal red phosphorus, the problem of safe storage and use of microcapsule red phosphorus, the problem of dark color of red phosphorus, and the problem that the particle size of common red phosphorus flame retardants is large, the red phosphorus flame retardants are difficult to uniformly disperse in high polymer materials, the flame retardant effect of the red phosphorus flame retardants is influenced, and the wide use of the red phosphorus flame retardants is hindered.
Magnesium hydroxide is an additive inorganic flame retardant for high polymer materials, and compared with other inorganic flame retardants, magnesium hydroxide has the following advantages: the magnesium hydroxide has triple functions of flame retardance, smoke abatement and filling, and endows the material with smoke-free and non-corrosive properties, and can obtain better flame retardance and smoke abatement effects; secondly, no harmful substance is discharged in the production, use and waste processes of the magnesium hydroxide, so that the environmental pollution is avoided; and (III) the initial thermal decomposition temperature of the magnesium hydroxide is 340 ℃, the decomposition is complete at 490 ℃, and the decomposition temperature is 140 ℃ higher than that of the aluminum hydroxide. Its total endotherm is 44.8KJ/mol, which is about 17% higher than the total endotherm of aluminum hydroxide. Therefore, the high-temperature-resistant and high-temperature-resistant composite material can bear higher processing temperature, is favorable for accelerating extrusion molding speed in product production and shortening molding time; the magnesium hydroxide can promote the carbon formation of the polymer to form a protective layer and exert better flame retardant effect besides self dehydration during combustion and decomposition; and (V) the magnesium hydroxide is matched with other flame retardants to show good flame-retardant synergistic effect. Therefore, in recent years, magnesium hydroxide has been highly regarded as a flame retardant and has been rapidly developed. At home and abroad, the magnesium hydroxide is consistently considered to be the main inorganic flame retardant. However, the common magnesium hydroxide flame retardant has large particles, is not easy to be uniformly dispersed in a high polymer material, and the magnesium hydroxide molecules have strong polarity and poor compatibility with the high polymer material, so that the mechanical property of the flame retardant material is sharply reduced. Currently, the method for solving the problem is to refine magnesium hydroxide particles to prepare micron powder, submicron powder or nanometer powder. The nanometer magnesium hydroxide has better flame retardant and smoke abatement effects than micron and industrial micron powder, and particularly has better filling and reinforcing effects, thus being one of the important directions for the development of flame retardants.
The red phosphorus and the magnesium hydroxide are used as the flame retardant, and the obvious flame retardant synergistic effect is achieved, because the magnesium hydroxide is dehydrated at high temperature, the red phosphorus is fully converted into phosphoric acid and polymetaphosphoric acid. The strong dehydration of polymetaphosphoric acid in turn promotes the magnesium hydroxide dehydration reaction to proceed more thoroughly. Through mutual promotion, the flame retardant performance of the two materials is fully exerted, the dehydration heat absorption and carbon formation heat insulation and oxygen isolation effects are enhanced, and an excellent synergistic effect is shown. The red phosphorus is used as a flame retardant together with aluminum hydroxide and zinc borate, and has the samesynergistic effect. If the red phosphorus is compounded with magnesium hydroxide, aluminum hydroxide, zinc borate and the like in an ultramicro state to prepare the ultramicro red phosphorus composite flame retardant, the synergistic effect of the red phosphorus and the magnesium hydroxide, the aluminum hydroxide, the zinc borate and the like can be more fully exerted.
At present, the red phosphorus flame retardant is mainly sold on the market in a microcapsule form and has a large particle size. In the last year, Wuhan Hengxin Bortai Business company Limited collaborated with the domestic research units to develop a red phosphorus flame retardant, UNICON-P, the surface of which was modified by organic matter and the minimum particle size of which was 1500 meshes. The Chinese science and technology university discusses the flame retardant property of Microencapsulated Red Phosphorus (MRP) in Magnesium Hydroxide (MH) flame retardant Low Density Polyethylene (LDPE), and the result shows that the oxygen index of the flame retardant material can be effectively improved by adding a proper amount of MRP in a LDPE/MH system. The Beijing university of chemical industry develops the synergistic flame retardant technology of nano magnesium hydroxide low filling and red phosphorus, and the synergistic flame retardant technology is successfully used for manufacturing flame retardant electric wires and cables. The currently used red phosphorus/magnesium hydroxide flame retardants have the following problems: red phosphorus, including microencapsulated red phosphorus, exists unsafe factors; the particle sizes of the red phosphorus and the microcapsule red phosphorus are large, so that the red phosphorus and the microcapsule red phosphorus are not beneficial to uniform dispersion in matrixes such as high polymer materials and the like, and the flame-retardant synergistic effect is difficult to fully exert; thirdly, each component of the synergistic flame retardant, red phosphorus, magnesium hydroxide or aluminum hydroxide and the like exist independently, so that the consistency of each batch of formula is difficult to ensure, two or more solid components are difficult to be uniformly mixed and uniformly dispersed in a matrix, and the full play of the flame retardant synergistic effect is influenced; and (IV) red phosphorus, including microcapsule red phosphorus, is dark red, and the application range of the red phosphorus is seriously influenced. The market requires a whiteness-oriented light-color ultramicro red phosphorus composite flame retardant.
The inventor of Yangdong province Zhongshan City patent application Yangdian has filed for the invention patent of 'manufacturing method and product of magnesium hydroxide loose nano particle block fire retardant', application number: 200510033253.X, application date: 23/2/2005, publication No.: CN1667029, published: 9/14/2005. On the basis, further research is carried out to develop and develop a bubble liquid film method for manufacturing the ultramicro red phosphorus composite flame retardant and the product.
[ summary of the invention]
The invention aims to provide a bubble liquid membrane method for manufacturing an ultramicro red phosphorus composite flame retardant and a product, which adopts a bubble liquid membrane reactor with a bubble disk type stirrer, takes one, two or more than two aqueous solutions of water-soluble salts, oxides or hydroxides of magnesium, aluminum, calcium, zinc and silicon elements as raw materials, and uses NaOH and NH3-H2O、NH3、Ca(OH)2、Na2CO3、(NH4)2CO3、NaHCO3、H2SO4、H3BO3Or CO2One, two or more than two aqueous solutions or gases are used as a settling agent, red phosphorus is dispersed into ultramicro red phosphorus particles in a raw material aqueous solution or a settling agent aqueous solution, and fatty acid (salt), polyunsaturated fatty acid (salt), titanate, silicate ester and sulfonic acid are used for preparing the ultrafine red phosphorus particlesEster, sulfate, phosphate, or titanate, silicate, sulfonate, sulfate, phosphate with at least one hydroxyl group (OH) in the central atom of Ti, Si, S, P, or salt solution converted into salt in the reaction system, with one, two or more of them being surface modifier, to prepare the composite flame retardant. According to a continuous, semi-continuous or intermittent process, gas is introduced into a bubble liquid membrane reactor, sufficient bubble flow is generated in a reaction system by utilizing the powerful gas charging function of a bubble disk type stirrer and the homogenization, dispersion and emulsification effects, the reaction liquid is divided into liquid membranes by the bubbles, the bubbles are dispersed phases, the liquid membranes are continuous phases, and a nano, submicron and/or micron reaction environment is formed. The reactants react in the liquid film to generate ultrafine particles (nanoparticles, submicron particles, micron particles less than or equal to 100 mu m) of water-insoluble or water-insoluble hydroxides, oxides or salts of magnesium, aluminum, calcium and silicon elements. The ultrafine particles completely or partially coat the surfaces of the ultrafine red phosphorus particles dispersed in the liquid film to form ultrafine red phosphorus composite particles. The nonpolar part of the surface modifier in the reaction system extends into the bubbles to absorb enough gas, the polar part extends into the liquid film, and is combined with the surface of the generated ultramicro red phosphorus composite particles at the interface of the bubbles and the liquid film to be coated in situ to form a coating layer, so as to generate the ultramicro red phosphorus composite capsule particles. Sufficient gas is adsorbed from the bubbles on the surfaces of the ultramicro red phosphorus composite particles and the ultramicro red phosphorus composite capsule particles to form a gas phase interface, so that the agglomeration of the ultramicro red phosphorus composite particles and the ultramicro red phosphorus composite capsule particles is inhibited, and simultaneously, the formation of hydrogen bond bridges among water molecules among the ultramicro red phosphorus composite particles, the ultramicro red phosphorus composite capsule particles or the ultramicro red phosphorus composite capsule particles is prevented, and the hydrogen bond combination among the particles is inhibited. Because enough gas exists among the particles, foam products are generated, and the ultramicro red phosphorus composite flame retardant is prepared after separation, washing and drying. This is achieved byThe ultramicro red phosphorus composite flame retardant has the appearance color obviously lighter than the color of red phosphorus, is pink or grey white powder, block or loose block, and has the internal components that in a three-dimensional space, at least one dimension is in the range of 1nm-100nm, or the nanometer capsule particle coated by a surface modifier, and the particle diameter is 100nm-1 mu, or the submicron particle coated by the surface modifierSubmicron capsule particles and micron particles with the particle size of 1-100 mu m or micron capsule particles coated by surface modifier.
The steps adopted for realizing the invention are as follows:
firstly, raw materials:
1. red phosphorus
The general molecular formula is as follows: p4
Producing land: purchased from Guangzhou
2. Magnesium chloride
The general molecular formula isas follows: MgCL2·6H2O
Producing land: purchased from Guangzhou
3. Settling agent
(1) Aqueous ammonia
The molecular formula is as follows: NH (NH)3·H2O
Producing land: purchased from Guangzhou
(2) Sodium hydroxide
The molecular formula is as follows: NaOH
Producing land: purchased from Guangzhou
4. Surface modifier
(1) Fatty acid ammonium salt
The general molecular formula is as follows: RCOONH4R is a hydrocarbyl or substituted hydrocarbyl group
Producing land: applied chemistry research institute of Zhongshan City
(2) Fatty acid sodium salt
The general molecular formula is as follows: RCOONa R is alkyl or substituted alkyl
Producing land: applied chemistry research institute of Zhongshan City
II, chemical reaction equation:
reaction equipment, steps and mechanism
Reaction equipment:
(1) the name and the model number are as follows: NA-1 intermittent bubble liquid film reactor
Producing land: applied chemistry research institute of Zhongshan City
(2) The name and the model number are as follows: NA-2 type continuousbubble liquid film reactor
Producing land: applied chemistry research institute of Zhongshan City
(II) reaction steps and mechanism:
adopts a bubble liquid film reactor with a bubble disk type stirrer, takes one, two or more than two aqueous solutions of water-soluble salts, oxides or hydroxides of magnesium, aluminum, calcium, zinc and silicon elements as raw materials, and uses NaOH and NH3-H2O、NH3、Ca(OH)2、Na2CO3、(NH4)2CO3、NH4HCO3、H2SO4、H3BO3Or CO2One, two or more than two aqueous solutions or gases are used as a settling agent, red phosphorus is dispersed into ultramicro red phosphorus particles in a raw material aqueous solution or a settling agent aqueous solution, and the ultramicro red phosphorus particles are converted into salt by using a fatty acid (salt), a polyunsaturated fatty acid (salt), titanate, silicate ester, sulfonate, sulfate, phosphate, or a titanate, silicate ester, sulfonate, sulfate and phosphate which have at least One Hydroxyl (OH) on central atoms of Ti, Si, S and P, or are converted into salt in a reaction system, wherein one, two or more than two are used as surface modifiers. According to the continuous, semi-continuous or intermittent process, gas is introduced into a bubble liquid membrane reactor, sufficient bubble flow is generated in a reaction system by utilizing the powerful gas charging function of a bubble disk type stirrer and the homogenization, dispersion and emulsification effects, the reaction liquid is divided into liquid membranes by the bubbles, the bubbles are dispersed phases, the liquid membranes are continuous phases, and a nano, submicron and/or micron reaction environment is formed. The reactants are inThe reaction is carried out in the liquid film togenerate ultrafine particles (nanoparticles, submicron particles, particles with the diameter less than or equal to 100 mu m) of water-insoluble or water-insoluble hydroxides, oxides or salts of magnesium, aluminum, calcium and silicon elements. The ultrafine particles completely or partially coat the surfaces of the ultrafine red phosphorus particles dispersed in the liquid film to form ultrafine red phosphorus composite particles. The nonpolar part of the surface modifier in the reaction system extends into the bubbles to absorb enough gas, the polar part extends into the liquid film, and is combined with the surface of the generated ultramicro red phosphorus composite particles at the interface of the bubbles and the liquid film to form a coating layer by in-situ coating, so as to generate the ultramicro red phosphorus composite capsule particles. Sufficient gas is adsorbed from the bubbles on the surfaces of the ultramicro red phosphorus composite particles and the ultramicro red phosphorus composite capsule particles to form a gas phase interface, so that the agglomeration of the ultramicro red phosphorus composite particles and the ultramicro red phosphorus composite capsule particles is inhibited, and simultaneously, the formation of hydrogen bond bridges among water molecules among the ultramicro red phosphorus composite particles, the ultramicro red phosphorus composite capsule particles or the ultramicro red phosphorus composite capsule particles is prevented, and the hydrogen bond combination among the particles is inhibited. Because enough gas exists among the particles, foam products are generated, and the ultramicro red phosphorus composite flame retardant is prepared after separation, washing and drying. The appearance of the ultramicro red phosphorus composite flame retardant is pink or grey powder, block or loose block, the color of which is obviously lighter than the color of red phosphorus, and the ultramicro red phosphorus composite flame retardant has the internal components that in a three-dimensional space, at least one dimension of nano particles or nano capsule particles coated by a surface modifier is in the range of 1nm-100nm, submicron particles or submicron capsule particles coated by the surface modifier with the particle size of 100nm-1 mu, and micron particles or micron capsule particles coated by the surface modifier with the particle size of 1 mu m-100 mu m.
Fourthly, the invention has the following advantages:
the bubble liquid membrane reactor has powerful gas filling, dispersing, homogenizing and emulsifying functions, and the reaction liquid is separated into liquid membrane with controllable size and narrow distribution. The equipment is exquisite, the cost is low, the labor is simple and concise, the process is smooth, and the large-scale production can be implemented;
the superfine red phosphorus particles are coated with superfine water insoluble or water insoluble hydroxide, oxide or salt of Mg, Al, Ca and Si elements and surface modifier to produce superfine red phosphorus composite fire retardant. The product is not a simple mixture of two or more components. The composite product can fully exert the flame-retardant synergistic effect of red phosphorus, has good compatibility with high polymer material molecules, is favorable for uniform dispersion, and is safe to transport, store and convenient to use;
compared with the red phosphorus or microcapsule red phosphorus, the ultramicro red phosphorus composite flame retardant has much lighter color, is pink or grey white, and greatly increases the application range of the product.
[ description of the drawings]
The manufacturing process and product of the present invention will be further illustrated by the following description and specific embodiments in conjunction with the accompanying drawings.
FIG. 1 is a flow chart of the method for preparing the ultramicro red phosphorus composite flame retardant and the product by the bubble liquid film method.
[ detailed description]according to the present embodiment
Example 1:
dispersing required amount of red phosphorus in 20mol of sodium hydroxide aqueous solution at 20-35 ℃ to obtain suspension of ultramicro red phosphorus particles, adding the suspension into a Na-1 type intermittent bubble liquid membrane reactor, starting stirring, introducing air to ensure that all reaction liquid is uniformly filled with micro bubbles, slowly adding 10mol of magnesium chloride aqueous solution into a reaction system until the pH value is 10-10.5, stirring for 5-15min, then adding sodium aliphatate aqueous solution, stirring for 20-30min, stopping reaction, floating a foam product on the upper layer of the reaction system, separating, washing with water, and drying in vacuum to obtain the grey ultramicro red phosphorus composite flame retardant. The product is detected to have the grain diameter of 90 percent to 40 nm.
Example 2:
at 20-35 deg.C, the required amount of red phosphorus is put in 2000cm3(25-27%) ammonia water is dispersed into ultramicro red phosphorus particles to form suspension, then the suspension is added into Na-1 type intermittent bubble liquid membrane reactor, stirring is startedStirring, introducing air to uniformly fill fine bubbles in the whole reaction solution, and chlorinating 10molSlowly adding the magnesium aqueous solution into the reaction system until the pH value is 10-10.5, stirring for 5-15min, adding the fatty acid ammonium aqueous solution, stirring for 20-30min, stopping reaction, floating the foam product on the upper layer of the reaction system, separating, washing with water, and drying in vacuum to obtain the gray ultramicro red phosphorus composite flame retardant. The product has 80% of particle size and 80nm by detection.
Example 3:
introducing air at the temperature of 20-35 ℃, starting a stirrer, dispersing a magnesium chloride aqueous solution with the concentration of 2mol and red phosphorus in a sodium hydroxide aqueous solution with the concentration of 4mol into a suspension of ultramicro red phosphorus particles and a sodium aliphatate aqueous solution with the concentration of 0.2mol by using a metering pump, adding the suspension and the sodium aliphatate aqueous solution into a Na-2 type continuous bubble liquid membrane reactor in a concurrent flow manner for reaction, controlling the pH of an effluent foamy reaction product to be 10-10.5, and filtering, washing and drying to obtain the off-white ultramicro red phosphorus composite flame retardant. The product has the particle size of 70 percent 80nm by detection.
Claims (3)
1. The method for preparing ultramicro red phosphorus composite fire retardant and its product by bubble liquid film method is characterized by that it uses one or two or more aqueous solutions of water-soluble salt, oxide or hydroxide of magnesium, aluminium, calcium, zinc and silicon elements as raw material, and uses NaOH and NH as raw material3-H2O、NH3、Ca(OH)2、Na2CO3、(NH4)2CO3、NaHCO3、H2SO4、H3BO3Or CO2One, two or more than two aqueous solutions or gases are used as a settling agent, red phosphorus is dispersedinto ultramicro red phosphorus particles in a raw material aqueous solution or a settling agent aqueous solution, and the ultramicro red phosphorus particles are prepared by using one, two or two of salts of fatty acid (salt), polyunsaturated fatty acid (salt), titanate, silicate, sulfonate, sulfate, phosphate, or titanate, silicate, sulfonate, sulfate and phosphate with at least One Hydroxyl (OH) on central atoms of Ti, Si, S and P, or salts of titanate, silicate, sulfonate, sulfate and phosphate which are converted into corresponding salts in a reaction systemThe above is surface modifier, the ultramicro red phosphorus composite flame retardant is prepared:
introducing gas into a bubble liquid film reactor with a bubble cap disc type stirrer, generating enough bubble flow in a reaction system by utilizing the powerful gas charging function of the bubble cap disc type stirrer and homogenizing, dispersing and emulsifying effects, dividing the reaction liquid into liquid films by the bubbles, wherein the bubbles are dispersed phases, and the liquid films are continuous phases to form nano, submicron and/or micron reaction environments, reacting reactants in the liquid films to generate superfine particles of water-insoluble or water-insoluble hydroxides, oxides or salts of magnesium, aluminum, calcium and silicon elements, and coating the superfine red phosphorus particles dispersed in the liquid films to generate superfine red phosphorus composite particles;
(II) using a fatty acid (salt), a polyunsaturated fatty acid (salt), a titanate, a silicate, a sulfonate, a sulfate, a phosphate, or a salt water solution of the titanate, the silicate, the sulfonate, the sulfate, the phosphate, or the titanate, the sulfonate, the sulfate, the phosphate, which at least has One Hydroxyl (OH) on a central atom of Ti, Si, S, P, or converting into a corresponding salt in a reaction system as a surface modifier, wherein the non-polar part of the surface modifier extends into the air bubbles to absorb a sufficient amount of gas, the polar part extends into the liquid film, and is combined with the surface of the generated ultramicro red phosphorus composite particles at the interface of the air bubbles and the liquid film to form a coating layer by in-situ coating to form the ultramicro red phosphorus composite capsule particles;
(III) adsorbing enough gas from bubbles on the surfaces of the generated ultramicro red phosphorus composite particles and ultramicro red phosphorus composite capsule particles to form a gas phase interface, inhibiting the agglomeration of the ultramicro red phosphorus composite particles or the ultramicro red phosphorus composite capsule particles, and simultaneously inhibiting water molecules from forming hydrogen bond bridges between the ultramicro red phosphorus composite particles or between the ultramicro red phosphorus composite particles to inhibit the hydrogen bond bonding between the ultramicro red phosphorus composite capsule particles or between the ultramicro red phosphorus composite particles and the ultramicro red phosphorus composite capsule particles, and generating a foam product due to the existence of enough gas between the particles, and separating, washing and drying to obtain the ultramicro red phosphorus composite particles or/and ultramicro red phosphorus composite capsule particle powder, blocks or/and loose blocks of hydroxides, oxides or salts of magnesium, aluminum, calcium, zinc and silicon elements on the surfaces of the ultramicro red phosphorus composite particles, namely the ultramicro red phosphorus composite flame retardant;
and (IV) the prepared ultramicro red phosphorus composite flame retardant product is a block or powder or loose block with the color obviously lighter than that of red phosphorus in appearance, and consists of ultramicro red phosphorus composite particles or ultramicro red phosphorus composite capsule particles, wherein the particle size of the ultramicro red phosphorus composite particles or ultramicro red phosphorus composite capsule particles is in a three-dimensional space, and at least one dimension of the nanometer particles or the nanometer capsule particles coated by a surface modifier is in a range of 1nm to 100nm, the submicron particles or the micron capsule particles coated by the surface modifier is in a range of 100nm to 1 mu m, or/and the micron particles or the micron capsule particles coated by the surface modifier is in a range of 1 mu m to 100 mu m.
2. The method of claim 1, wherein the gas is introduced into the bubble liquid membrane reactor, and the raw material aqueous solution or the sedimentation agent aqueous solution or the gas, the surface modifier (aqueous solution) and the red phosphorus are dispersed into the ultramicro red phosphorus particles in the raw material aqueous solution or the sedimentation agent aqueous solution, and are added into the bubble liquid membrane reactor in parallel, and the ultramicro red phosphorus composite particles are generated in the formed liquid membrane and are coated in situ to generate the ultramicro red phosphorus composite capsule particles; according to an intermittent or semi-continuous process, firstly dispersing raw material aqueous solution or settling agent aqueous solution (or gas) and red phosphorus in the raw material aqueous solution or settling agent aqueous solution to obtain ultramicro red phosphorus particle suspension, adding the ultramicro red phosphorus particle suspension into a bubble liquid film reactor, firstly preparing ultramicro red phosphorus composite particles, then adding a surface modifier (aqueous solution) into a reaction system, and coating to generate ultramicro red phosphorus composite capsule particles; or the reaction mixture which has generated the ultramicro red phosphorus composite particles enters a secondbubble liquid film reactor, and then a surface modifier (aqueous solution) is added into the reaction system for coating to generate the ultramicro red phosphorus composite capsule particles; according to the requirement, secondary or multiple coating can be carried out; if necessary, separating the ultramicro red phosphorus composite particles or the ultramicro red phosphorus composite capsule particles, and then coating for one time, two times or more to generate the ultramicro red phosphorus composite flame retardant product.
3. The method for preparing ultra-fine red phosphorus composite flame retardant and product according to claim 1, wherein the ultra-fine red phosphorus composite flame retardant is prepared by completely or partially coating the surfaces of ultra-fine red phosphorus particles with ultra-fine particles of hydroxides, oxides or salts of magnesium, aluminum, calcium, zinc and silicon and ultra-fine capsule particles to form ultra-fine red phosphorus composite particles and/or ultra-fine red phosphorus composite capsule particle powder, blocks or loose blocks, which are pink or grey white. The color of the product is lighter than that of red phosphorus itself or red phosphorus microcapsules in general.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182052B (en) * | 2007-11-16 | 2012-07-18 | 曾能 | Treatment of alkaline black liquor by bubble liquid membrane bittern method |
| CN103825002A (en) * | 2014-01-29 | 2014-05-28 | 浙江工业大学 | Composite material using titanium dioxide as skeleton structure to clad phosphorus and application of composite material |
-
2006
- 2006-02-16 CN CN 200610033637 patent/CN1824730A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182052B (en) * | 2007-11-16 | 2012-07-18 | 曾能 | Treatment of alkaline black liquor by bubble liquid membrane bittern method |
| CN103825002A (en) * | 2014-01-29 | 2014-05-28 | 浙江工业大学 | Composite material using titanium dioxide as skeleton structure to clad phosphorus and application of composite material |
| CN103825002B (en) * | 2014-01-29 | 2017-01-04 | 浙江工业大学 | It is composite and the application thereof that framing structure is coated with phosphorus with titanium dioxide |
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