CN1181385A - Method for synthetizing triphenyl tin acetate - Google Patents

Abstract

A process for synthesizing tin triphenylacetate features the on-step syntehsis from tin triphenylchloride and anhydrous sodium acetate. Its advantages include short reaction time, simple process, high productivity and ouput rate, less consumption of solvent (mixture solution of tuluene and isopropanol), and low requirement to apparats.

Description

Novel method for synthesizing triphenyl tin acetate

The invention relates to a method for synthesizing triphenyl tin acetate by using triphenyl tin chloride and anhydrous sodium acetate as raw materials through a one-step method.

Triphenyltin acetate, which is commonly known as distemper tin potato, is a protective bactericide produced by Hoechst of Germany at present and generally adopts two stepsThe method is synthesized, and the balance formula is as follows:

firstly Ph₃Conversion of SnCl to Ph₃SnOH related documents:

Japan KoKai76.16.646(Cl C07F7/22)10.Feb.1976

Japan KoKai 77.113.950(Cl C07F7/22)24.Sep.1977

then Ph₃SnOH reacts with iced HAC to synthesize Ph₃SnAC, related literature:

J.APPl CHem 1956(6)56

pol 51.771(Cl co7f) oct.15.1966. two-step synthesis of triphenyltin acetate is characterized by using triphenyltin chloride (Ph)₃SnCl) and sodium hydroxide (NaOH) to obtain triphenyltin hydroxide (Ph)₃SnOH) and waste residue sodium chloride (NaCl), methanol is used as solvent; followed by triphenyl tin hydroxide (Ph)₃SnOH) as raw material reacts with acetic acid (HAC) to generate triphenyl tin acetate, and waste liquid is discharged, and hexane is used as solvent. The method has the disadvantages of long reaction route and time, complex process route, large equipment investment, low production capacity and yield, large solvent consumption and high cost due to long reaction time because the two-step synthesis method adopts the solvents AAlcohol, hexane and raw materials except triphenyltin chloride comprise six raw materials of sodium hydroxide, acetic acid and self-synthesized intermediate triphenyltin hydroxide, the boiling point of methanol is low by 65 ℃, the toxicity is high, the boiling point of hexane is 68 ℃ and is volatile, NaOH is strong in alkali, the corrosivity is high, acetic acid has strong pungent odor, the requirements on process control conditions and equipment are high, purchasing and storage are difficult, water in the two-step method is a product after reaction and contains a plurality of reaction elements such as organic solvents, element tin and the like, the toxicity is high, the pollution is serious after the discharge, and the treatment is difficult.

The invention aims to provide a reaction route with short time compared with a two-step synthesis method aiming at the defects of the two-step synthesis method for synthesizing the triphenyl tin acetate; the process route is simple, and the equipment investment is relatively small; the production capacity and the yield are high; the solvent consumption is less and the cost is low; the raw materials have low requirements on the process and equipment, and are easy to purchase and store; the method for synthesizing the triphenyl tin acetate by a one-step method has no pollution to emissions and is easy to treat.

The technical scheme of the invention is as follows: under the anhydrous condition, adding 0.5-1 part of toluene, 2-7 parts of isopropanol, 1-8 parts of triphenyltin chloride and 0.5-3 parts of anhydrous sodium acetate into a reaction kettle, starting the reaction kettle for stirring, simultaneously opening a steam heating valve of a jacket of the reaction kettle to heat the reaction kettle to the temperature of 60-100 ℃, keeping the temperature range for 2-5 hours, stopping stirring, putting the material into a filter pressing tank heated to the temperature of 60-90 ℃ by steam, pressurizing the filter pressing tank to 0.2MPa, keeping the pressure for filter pressing for 2-6 hours, pressing the material into a cooling crystallization tank, stirring, cooling the filter pressing tank to room temperature, taking out residues (the main component is NaCl) on a filter cloth layer in the filter pressing tank, reducing the temperature of the material in the cooling crystallization tank to 30-10 ℃ when the filter pressing is finished, stopping stirring, standing for 2-4 hours, putting the materials into a filter tank, filtering out the mixed solvent of toluene and isopropanol for recycling,taking out the triphenyl tin acetate tray, and putting the triphenyl tin acetate tray into a drying chamber with the temperature of 60-80 ℃ for drying until the heating loss is less than 1%. Adding filler into the prepared triphenyl tin acetate according to a certain proportion, carrying out superfine grinding and superfine grinding, and mixing to prepare wettable powder containing 10-90% of triphenyl tin acetate. One-step method is balanced as

Compared with the existing method for synthesizing the triphenyl tin acetate by the two-step method, the method has the advantages that the reaction route of the one-step method is half of that of the two-step method, the reaction time is half of that of the two-step method, the one-step method is simpler than the two-step method, the required reaction equipment and production line only need half of that of the two-step method, the equipment investment is saved, and the production capacity is doubled; the total yield of the one-step method can be more than 90 percent, and the total yield of the two-step method is only 80 percent if each step is 90 percent, because the reaction time of the one-step method is short, the solvent consumption can be saved by 1/5 compared with the two-step method, the cost is reduced by more than 20 percent, the one-step method only uses four raw materials which are much easier to purchase and store than the two-step method, and the solvent in the raw materials is toluene, the boiling point is 110.6 ℃ and is low in toxicity, the boiling point of isopropanol is 82.3 ℃ and is nontoxic, and NaAC solid is tasteless, nontoxic and stable, because the used solvent is a mixed solvent of toluene and isopropanol, the boiling point is about 100 ℃, the stability is good, the toxicity is.

The attached figure is a process block diagram of a new method for synthesizing the triphenyl tin acetate.

The preferred embodiments of the present invention are given below with reference to the accompanying drawings: under the anhydrous condition, adding 0.5-1 part of toluene, 2-7 parts of isopropanol, 1-8 parts of triphenyl tin chloride and 0.5-3 parts of anhydrous sodium acetate into a reaction kettle, starting the reaction kettle for stirring, simultaneously opening a steam heating valve of a jacket of the reaction kettle to heat the reaction kettle, heating to 60-100 ℃, keeping the temperature for reaction for 2-5 hours, stopping stirring, putting the materials into a filter pressing tank which is heated to 60-90 ℃ by steam in advance, starting an air pump, simultaneously opening an air inlet valve of the filter pressing tank, keeping the pressure in the filter pressing tank at 0.2MPa for filter pressing for 2-6 hours, pressing the materials into a cooling crystallization tank and stirring, after the filter pressing is finished, opening a cooling water valve of the filter pressing tank to reduce the temperature of the filter pressing tank to room temperature, then opening a hand hole of the filter pressing tank, taking out residues (the main component is NaCl) on a filtercloth layer by using a climbing iron, opening a cold brine inlet and outlet valve of the cooling crystallization tank to reduce the temperature of the materials in the cooling crystallization tank to 30-10 ℃ when the filter pressing is finished, stopping stirring, standing for 2-4 hours, putting the materials into a filter tank, starting a water ring vacuum pump to pump the filtered toluene and isopropanol mixed solvent into a recovery tank for recycling, opening a hand hole of the filter tank after the filtering is finished, taking out the triphenyl tin acetate by using a crawler, putting the triphenyl tin acetate into a square plate, and drying the square plate in a drying chamber at 60-80 ℃ until the heating loss is less than 1%. The prepared triphenyl tin acetate is added with filler to prepare wettable powder containing 10 to 90 percent of triphenyl tin acetate.

Claims (1)

1. A new method for synthesizing triphenyl tin acetate is characterized in that: under the anhydrous condition, adding 0.5-1 part of toluene, 2-7 parts of isopropanol, 1-8 parts of triphenyltin chloride and 0.5-3 parts of anhydrous sodium acetate into a reaction kettle, starting the reaction kettle for stirring, simultaneously opening a steam heating valve of a jacket of the reaction kettle to heat the reaction kettle to the temperature of 60-100 ℃, keeping the temperature range for 2-5 hours, stopping stirring, putting the material into a filter pressing tank heated to the temperature of 60-90 ℃ by steam, pressurizing the filter pressing tank to 0.2MPa, keeping the pressure for filter pressing for 2-6 hours, pressing the material into a cooling crystallization tank, stirring, cooling the filter pressing tank to room temperature, taking out residues on a filter cloth layer in the filter pressing tank, reducing the temperature of the material in the cooling crystallization tank to 30-10 ℃ when the filter pressing is finished, stopping stirring, standing for 2-4 hours, putting the materials into a filter tank, filtering out the mixed solvent of toluene and isopropanol for recycling, taking out the triphenyl tin acetate, loading into a tray, putting into a drying chamber at the temperature of 60-80 ℃, drying until the heating loss is less than 1%, adding a filler into the prepared triphenyl tin acetate in proportion, carrying out ultrafine grinding and fine grinding, and mixing to prepare wettable powder containing 10-90% of triphenyl tin acetate.