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Preparation process of nano concave soil base inorganic flame-retarded agent

A technology of inorganic flame retardants and attapulgite, which is applied in the field of preparation of composite inorganic flame retardants, can solve problems such as uneven dispersion, product loss, and low separation efficiency, so as to increase filtration speed, improve flame retardant effect, and reduce loss rate effect

Inactive Publication Date: 2009-07-08
JIANGSU POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has two disadvantages: first, mechanical mixing generally has the problem of uneven dispersion, and cannot fully exert the synergistic effect between flame retardants; second, because the natural palygorskite is only crushed to 100-5000 mesh, only It belongs to the coarse crushing and rough processing of attapulgite, and does not disperse attapulgite aggregates into attapulgite nano single crystals
Due to the finer particles of attapulgite, there will be the following problems in solid-liquid separation: If filter cake filtration is used, due to the restriction of the filter medium, the interception effect on nano-attapulgite is poor, and the product loss is serious
High energy consumption and low separation efficiency caused by centrifugal separation
At present, the solid-liquid separation of nano-attapulgite is still a bottleneck restricting its large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Add natural attapulgite minerals into deionized water dissolved with 3% sodium polypropionate (mass ratio to attapulgite) to prepare a suspension containing attapulgite 120 g / L, ultrasonically disperse for 2 hours, and let stand for 24 hours; Adjust the pH value of the obtained upper nano-attapulgite dispersion to 9.5, raise the temperature to 100 ° C, and add 0.6 mol L dropwise to the nano-attapulgite dispersion while stirring. -1 Aqueous solution of sodium aluminate and 0.6mol·L -1 dilute sulfuric acid, maintain the reaction temperature at 100 ° C, pH = 9.0 ~ 10.0, dropwise add 40% of the mass of attapulgite within 1 hour (as Al 2 o 3 After dripping, adjust the pH=7.0 with dilute sulfuric acid, mature for 0.5h, put the feed liquid into the settling tank and let it stand for 2 days, and separate the clear water layer of the upper layer from the attapulgite thick slurry of the lower layer; The nano-attapulgite thick slurry obtained by sedimentation and sepa...

Embodiment 2

[0020] Embodiment 2: The natural attapulgite mineral is added into the deionized water that is dissolved with 3% sodium polypropionate (mass ratio with attapulgite), is mixed with the suspension containing attapulgite 80g / L, disperses at high speed with emulsifier for 4h, static Set it aside for 24 hours; adjust the pH value of the obtained upper nano-attapulgite dispersion to 9.5, raise the temperature to 40°C, and add 0.4mol·L dropwise to the nano-attapulgite dispersion while stirring. -1 Aluminum sulfate aqueous solution and 1.2mol·L -1 dilute ammonia water, maintain the reaction temperature at 40 ° C, pH = 9.0 ~ 10.0, within 5 hours, dropwise add 500% of the attapulgite mass (as Al 2 o 3 After dripping, adjust the pH=7.0 with dilute sulfuric acid, mature for 0.5h, put the feed liquid into the settling tank and let it stand for 1 day, separate the clear water layer of the upper layer from the attapulgite thick slurry of the lower layer; The separated nano-attapulgite thic...

Embodiment 3

[0021] Embodiment 3: Add the natural attapulgite mineral into the deionized water that is dissolved with 3% sodium polypropionate (mass ratio to attapulgite), and prepare a suspension containing attapulgite 60g / L, disperse at a high speed for 2h with an emulsifier, and statically Set it aside for 24 hours; adjust the pH value of the obtained upper nano-attapulgite dispersion to 9.5, raise the temperature to 70°C, and add 0.4mol·L dropwise to the nano-attapulgite dispersion while stirring. -1 Aluminum sulfate aqueous solution and 1.2mol·L -1 Sodium hydroxide aqueous solution, maintain reaction temperature 70 ℃, pH=9.0~10.0, drop within 5h and account for 200% of attapulgite quality (as Al 2 o 3After dripping, adjust the pH=7.0 with dilute sulfuric acid, mature for 0.5h, put the feed liquid into the settling tank and let it stand for 1 day, separate the clear water layer of the upper layer from the attapulgite thick slurry of the lower layer; The separated nano-attapulgite thi...

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Abstract

The invention relates to a method for preparing a composite inorganic flame retardant by taking nano attapulgite as a nucleus and coating the surface with Mg, Al, Sb and the like. It prepares the nano-attapulgite water dispersion into a suspension with a solid content of 10-200g / L, heats it to 40-100°C, and uses an inorganic flame retardant to carry out inorganic surface coating treatment on the nano-attapulgite under stirring. Nano-attapulgite surface coatings are one, two or more of Al2O3 hydrate, MgO hydrate, antimony oxide hydrate, ZnO hydrate, zinc borate, and stand still to make the inorganic surface-coated nano Attapulgite settles and separates from the suspension to achieve preliminary solid-liquid separation; after plate and frame filtration and washing, the washed nano-attapulgite filter cake is dried at 80-150°C; then pulverized to reduce nano-attapulgite base The degree of agglomeration of inorganic flame retardants. The attapulgite-based inorganic flame retardant prepared by the invention not only has the function of flame retardancy, but also has a good reinforcing effect.

Description

technical field [0001] The invention relates to a preparation method of a nano-attapulgite-based inorganic flame retardant, specifically a composite inorganic flame retardant that takes nano-attapulgite as a nucleus and coats the surface with Mg, Al, Sb, Zn, etc. Preparation. Background technique [0002] Flame retardant is an additive that makes polymers not easy to catch fire and slows down the burning speed after fire. It makes the material have the characteristics of flame retardancy, self-extinguishing and smoke suppression, and is one of the important additives for the processing of synthetic polymer materials. With the enhancement of people's awareness of environmental protection, the impact of flame retardant products on the environment has become the primary consideration in the selection of flame retardants. Halogenated flame retardants have been one of the important flame retardants for a long time. However, due to the release of toxic fumes when they burn, caus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K21/02
Inventor 姚超丁永红陈志刚李连惠李效棠李为民陈杨张良
Owner JIANGSU POLYTECHNIC UNIVERSITY
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