Preparation and application of tetrahydroxymethylphosphorus sulfate_Industrial additives

Background and overview[1][2]

Tetrahydroxymethylphosphorus sulfate (THPS) is mainly used as a bactericidal algaecide in water treatment, oil field pipelines, fishery breeding, etc. It can quickly degrade into completely harmless substances after use. It is also often used for flame retardant treatment of fabrics. Leather softening and paper making industries. Tetrahydroxymethylphosphorus sulfate is a green and environmentally friendly quaternary phosphate fungicide. The product has good water solubility, low freezing point, stable chemical properties, and long-term storage does not affect its quality. It is a new, excellent, efficient, broad-spectrum, low-toxicity, low-dose, low-foaming, environment-friendly fungicide that has strong killing properties against bacteria and algae. In 1995, it was approved by the U.S. EPA, which determined its toxicity classification to be zero, and was awarded the U.S. Green Chemistry Award. Tetrahydroxymethylphosphorus sulfate is also an internationally recognized permanent flame retardant for pure cotton and polyester-cotton fabrics. Because of its active hydroxymethyl group in its chemical structure, its reactive properties are active and can interact with many substances such as amines and phenols. It can form a polymer and can be used with some resin pre-shrunks during vinyl-retardant finishing, which can give cotton fabrics excellent flame retardant properties.

Preparation[3]

The preparation method of tetrahydroxymethylphosphorus sulfate of the present invention includes:

Add sulfuric acid and formaldehyde into the reaction kettle, turn on the gas-liquid circulation mixing reaction pump, add phosphine into the gas-liquid circulation mixing reaction pump, and absorb phosphorus through the gas-liquid circulation mixing reaction device at 50-60°C The phosphine that has not been completely absorbed enters the next gas-liquid circulation mixing reaction pump (the two gas-liquid circulation mixing reaction devices are the same, but are connected in series, which is more conducive to the utilization of phosphine), and passes through the middle The formaldehyde content is controlled and detected to determine the end point of the reaction. After the reaction is completed, the reaction is concentrated under reduced pressure to obtain tetrahydroxymethylphosphorus sulfate.

Apply [2]

Used to prepare an anti-insect coating containing tetrahydroxymethylphosphorus sulfate:

CN201810167415.6 discloses an insect-proof coating containing tetrahydroxymethyl phosphorus sulfate and its preparation method. The process combines bentonite, yellow collagen, phosphate ester, sodium carbonate, magnesium carbonate, phenolic resin, ethylene oxide, Raw materials such as silicon carbide, trehalose, chitosan, zinc sulfate, polyurethane, and tetrahydroxymethylphosphorus sulfate are respectively ground, stirred and dispersed, gradient heating vacuum sintering, ultrasonic homogeneous dispersion, pressurized mixing, packaging, sealing, etc. The steps prepare an insect-proof paint containing tetrahydroxymethylphosphorus sulfate. The prepared insect-proof paint containing tetrahydroxymethylphosphorus sulfate has stable insect-proof effect, is non-toxic and harmless, is environmentally friendly and safe, has certain fire-proof performance, and has good application prospects.

Includes the following steps:

(1) Add 4-10 parts of bentonite, 2-5 parts of xanthocollagen, 1-2 parts of phosphate ester, 2-5 parts of sodium carbonate, and 1-4 parts of magnesium carbonate into a three-roller grinder for cutting and grinding. The stirring speed is 100 rpm, the grinder power is 500W; hydroxyl acrylic resin

(2) Combine 5-10 parts of phenolic resin, 2-5 parts of ethylene oxide, 1-3 parts of silicon carbide, 1-2 parts of trehalose, 1-3 parts of chitosan, and 2-5 parts of zinc sulfate Add 1-4 parts of polyurethane and 1-4 parts of lubricant to a high-speed mixer for dispersion. Stir and mix for 20 minutes at a stirring speed of 1000 rpm. Then add 1-4 parts of polyurethane and 3-6 parts of tetrahydroxymethylphosphorus sulfate in sequence, and then stir at high speed. Increase the speed to 2000 rpm/pack and continue stirring for 30 minutes to obtain a stirred mixture;

(3) Inject the ground material of step (1), the mixture of step (2), 1-4 parts of stabilizer, and 2-4 parts of coupling agent into a vacuum sintering furnace for three-step sintering. First In the first step of sintering, the temperature is raised to 80-85°C at a heating rate of 2°C/min and kept for 15 minutes. In the second step of sintering, the temperature is raised to 120-125°C at a heating rate of 5°C/min and kept for 20 minutes. In the third step of sintering, the control temperature is 150°C. -160℃, keep warm for 8-12h;

(4) Inject the reaction slurry in step (3) into an ultrasonic disperser for ultrasonic uniform dispersion;

(5) Inject the reactants of step (4) into the internal mixer, then add the defoaming agent to perform a pressurized reaction;

(6) Inject the reactant of step (5) into the automatic vacuum filling machine, and carry out packaging, sealing and packaging to obtain the finished product.

Compared with the prior art, the beneficial effects of this invention are:

(1) An insect-proof coating containing tetrahydroxymethylphosphorus sulfate of the present invention and its preparation method combine bentonite, xanthocollagen, phosphate ester, sodium carbonate, magnesium carbonate, phenolic resin, ethylene oxide, silicon carbide , trehalose, chitosan, zinc sulfate, polyurethane, tetrahydroxymethyl phosphorus sulfate and other raw materials are prepared through grinding, stirring and dispersing, gradient heating vacuum sintering, ultrasonic homogeneous dispersion, pressure mixing, packaging, sealing and other steps. An anti-insect coating containing tetrahydroxymethylphosphorus sulfate was obtained. The prepared insect-proof paint containing tetrahydroxymethylphosphorus sulfate has stable insect-proof effect, is non-toxic and harmless, is environmentally friendly and safe, has certain fire-proof performance, and has good application prospects.

(2) The insect-proof coating containing tetrahydroxymethylphosphorus sulfate of the present invention has easy-to-obtain raw materials, simple process, is suitable for large-scale industrial application, and has strong practicability.

Main reference materials

[1] CN201110350201.0 Method for determination of formaldehyde content in tetrahydroxymethylphosphorus sulfate

[2] CN201810167415.6 An insect-proof coating containing tetrahydroxymethylphosphorus sulfate and its preparation method

[3] CN201110057949.1 A kind of preparation method of tetrahydroxymethylphosphorus sulfate

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