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Preparation process of odorless phosphate flame retardant

A preparation process, a technology for phosphate esters, applied in the directions of phosphorus organic compounds, compounds of elements of Group 5/15 of the periodic table, chemical/physical/physical chemical processes using energy, etc. The aldehyde deodorization process cannot effectively solve the problem of the odor of phosphate ester flame retardants, and achieves the effect of good separation of impurities, avoidance of side reactions and short residence time.

Pending Publication Date: 2022-05-13
淮安晨化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this invention does not have special process of removing aldehyde and removing odor, and the obtained product still has the unpleasant smell that aldehydes send out
[0008] None of the above processes can effectively solve the problem of odor in phosphate ester flame retardants. It is necessary to develop a preparation process for phosphate ester flame retardants that is odorless and has high product quality stability.

Method used

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  • Preparation process of odorless phosphate flame retardant
  • Preparation process of odorless phosphate flame retardant
  • Preparation process of odorless phosphate flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0035] When working, put 153.33kg of phosphorus oxychloride into the crude product synthesis kettle, add 3.5kg of catalyst titanium tetrachloride after nitrogen replacement, slowly raise the temperature to 42°C and start feeding propylene oxide, and control the reaction temperature at 42±2°C, The input amount of propylene oxide was 179.1kg. After the input of propylene oxide was completed, it was incubated at 42°C for 1 hour, then vacuumed to -0.095mPa and kept at -0.095mPa for 1 hour to obtain the crude product.

[0036] Transport the crude product to the alkaline washing tank and add lye with a mass concentration of 10%. After adjusting the pH of the crude product to 7.5, transport it to the washing tank and add 33.2kg of water. After washing for 1 hour, let it stand for liquid separation once, remove the upper layer of washing liquid, and keep the lower layer product. Then add 33.2kg of water, wash with water for 1 hour, then let stand to separate the liquid, remove the was...

Embodiment 2

[0039] Put 153.33 kg of phosphorus oxychloride into the crude product synthesis kettle, add 3.9 kg of catalyst aluminum trichloride after nitrogen replacement, slowly raise the temperature to 45°C and start feeding propylene oxide, control the reaction temperature at 45±2°C, the input of propylene oxide The volume is 179.1kg. After the input of propylene oxide, heat preservation and aging at 45°C for 1h, then vacuumize to -0.098mPa, and keep the vacuum condition of -0.098mPa for 1h to obtain the crude product.

[0040] The crude product is transported to the caustic washing tank to add lye with a mass concentration of 20%. After the pH of the crude product is adjusted to 7.3, it is transported to the washing tank and added with 33.2 kg of water. Remove the lower layer of product. Then add 66.4kg of water, wash with water for 1 hour, then let stand to separate the liquid, remove the washing liquid in the upper layer, and keep the product in the lower layer. The lower layer pro...

Embodiment 3

[0043] Put 153.33kg of phosphorus oxychloride into the crude product synthesis kettle, add 3.0kg of catalyst boron trifluoride after nitrogen replacement, slowly raise the temperature to 50°C and start feeding propylene oxide, control the reaction temperature at 50±2°C, the input of propylene oxide The weight is 179.1kg. After the propylene oxide input is completed, heat preservation and aging at 50°C for 1h, and then vacuumize to -0.100mPa or MPA, and maintain the vacuum condition of -0.100mPa for 1h to obtain the crude product.

[0044] Transport the crude product to the alkaline washing tank and add lye with a mass concentration of 25%, adjust the pH of the crude product to 7.5, then transport it to the washing tank and add 39.2kg of water, wash for 1 hour and then separate the liquid once, remove the upper layer of washing liquid, and keep the lower layer product. Then add 39.2kg of water, wash with water for 1 hour, then let stand to separate the liquid, remove the washin...

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Abstract

A preparation process of an odorless phosphate flame retardant belongs to the technical field of preparation of phosphate flame retardants, and comprises the following specific steps: sequentially performing the steps of crude product synthesis, alkali washing, water washing, activated carbon adsorption, ultrasonic oscillation, ultra-high-speed centrifugal molecular distillation and filter pressing to obtain the phosphate flame retardant. The method comprises the following steps: firstly, adsorbing aldehyde odor substances in a product by adopting activated carbon; secondly, an ultra-high-speed centrifugal molecular distillation device with a built-in ultrasonic oscillator is adopted to replace traditional dehydration equipment such as a kettle type or a film evaporator. The phosphate flame retardant prepared by the invention is colorless, transparent and odorless, the low acid value is less than or equal to 0.04 mgKOH / g, the low water content is less than or equal to 0.05%, and the low aldehyde content is less than or equal to 2ppm.

Description

technical field [0001] The invention belongs to the technical field of preparation of phosphate ester flame retardants, and in particular relates to a preparation process of an odorless phosphate ester flame retardant. Background technique [0002] Phosphate ester flame retardants are a class of organophosphorus flame retardants. Phosphate ester flame retardants mainly include tris(2-chloropropyl) phosphate (TCPP), tris(2-chloroethyl) phosphate (TCEP) , Tris(1,3-dichloropropyl) phosphate (TDCP), etc. [0003] Compared with other flame retardants, phosphate ester flame retardants have long-lasting flame retardant effects, good compatibility with polymers, water resistance, weather resistance, cold and heat resistance, and migration resistance. They are indispensable in the field of polymer materials such as polyurethane resins. The importance of substitution. Mainly used in polyurethane foam, polystyrene, epoxy resin, cellulose acetate, ethyl cellulose resin, unsaturated re...

Claims

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Application Information

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IPC IPC(8): C07F9/09C09K21/12B01D3/12B01D53/04B01J19/10
CPCC07F9/091C09K21/12B01J19/10B01D3/12B01D53/04
Inventor 贾正仁房连顺董晓红毕继辉郝银张杰陆国玲
Owner 淮安晨化新材料有限公司
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