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Preparation method of water-soluble tri(m-sulfonate phenyl)phosphine

A technology of triphenylphosphine and sulfonate, applied in the field of organic chemical synthesis, can solve the problems of easy corrosion and blockage of pipes, difficult control of gas flow rate, loss of TPPTS, etc., and achieves the effects of improving yield, easy control and simple operation.

Active Publication Date: 2013-08-21
成都欣华源科技有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] From the above technical background, the use of low concentration SO 3 When fuming sulfuric acid with a content of 20% is used as a sulfonating agent, there are more disulfonated and monosulfonated by-products in the sulfonated products of TPP, and SO 3 is the sulfonating agent, SO 3 The gas flow rate is not easy to control, adding SO 3 The pipeline is easily corroded and blocked, and the operation process is troublesome; when the sulfonated acid solution is neutralized with alkali, the amount of alkali is large, and the loss of TPPTS is caused when sodium sulfate is separated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]In a 500ml three-necked flask, add 300g of 100% concentrated sulfuric acid and 16g of sodium metaborate at a temperature of 25°C, stir until completely dissolved, cool the solution to 20°C, and then dissolve 70g of Under rapid stirring, triphenylphosphine was added to the three-necked flask in three batches within 1 hour. Nicotinic sulfuric acid, adjust the temperature to 35°C, react for 42 hours, after the solution is cooled to 5°C, add 500 ml of water to dilute, and then use 500 ml of toluene solution containing 50% triphenyl phosphite to extract the sulfonated product to organic layer, and then add sodium hydroxide to neutralize to pH = 8. After the solution is cooled to 5°C, filter to remove sodium sulfate, concentrate the collected mother liquor to about 200 ml under reduced pressure, and then cool the solution to below 5°C to make the residual Sodium sulfate was precipitated, and the solid was filtered out, and the filtrate was evaporated to dryness under reduced p...

Embodiment 2

[0034] Prepare TPPTS by the method for example 1, each raw material consumption is 400 grams of 100% vitriol oil, 20 grams of sodium metaborate, 70 grams of triphenylphosphine, 500 grams of oleum containing 50 weight % of sulfur trioxide, sulfonation reaction temperature 45°C, reaction time 46 hours, the reaction product was treated according to the method of Example 1 to obtain 141.3 g of sulfonated product, the yield was 93.0%, and the TPPTS content in the product was 95.1 mol%.

Embodiment 3

[0036] Prepare TPPTS by the method for example 1, each raw material consumption is 450 grams of 100% vitriol oil, 20 grams of sodium metaborate, 70 grams of triphenylphosphine, 450 grams of fuming sulfuric acid containing 60 weight % of sulfur trioxide, sulfonation reaction temperature 45 DEG C, reaction time 50 hours, reaction product is processed by the method for embodiment 1, obtains sulfonation product 138.3 grams, yield 92.1%, TPPTS content 95.8 mol% in the product

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Abstract

The invention relates to a preparation method of water-soluble tri(m-sulfonate phenyl)phosphine (TPPTS). The preparation method comprises the following steps of: adding sodium metaborate which is 1.5-20wt% of total reactants into 100% concentrated sulfuric acid, then adding triphenylphosphine in batches, stirring and dissolving; and then adding fuming sulphuric acid containing 50-60wt% of SO3, carrying out sulfonation reaction at a temperature of 25-45 DEG C for 38-58 hours, extracting a sulfonated product by using a toluene solution of phosphite ester; then adding an alkali solution to neutralize the product till the pH value is 8-9; and then separating and recycling the product, wherein in the reaction system, the molar ratio of the fuming sulphuric acid containing 50-60wt% of SO3 to the triphenylphosphine is 6-18, and the molar ratio of the concentrated sulfuric acid to the triphenylphosphine is 10-25. By adopting the preparation method, the operation is simple and easy to control, the reaction time is shortened, and the content of by-product oxides is reduced.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and relates to a preparation method of a water-soluble organic phosphine compound, in particular to a preparation method of a water-soluble tris(m-sulfonate phenyl)phosphine (TPPTS). Background technique [0002] In the 1950s, BP 1,066,261 and J. Chem. Soc. 276-288, 1958 reported that triphenylphosphine (hereinafter referred to as TPP) was sulfonated with oleum, and then neutralized with alkali solution to obtain the following formula: Water-soluble organophosphine compounds shown. [0003] [0004] where Ar 1 、Ar 2 、Ar 3 Can be the same or different, they represent aryl; Y 1 , Y 2 and Y 3 It can be the same or different, representing a straight chain or branched alkyl group containing 1 to 4 carbon atoms, an alkoxy group containing 1 to 4 carbon atoms, a halogen atom or a hydroxyl group, etc.; M represents an inorganic or organic cation; m 1 、m 2 and m 3 Can be the same or ...

Claims

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Application Information

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IPC IPC(8): C07F9/50
Inventor 李贤均陈锴陈华黎耀忠袁茂林王晓光
Owner 成都欣华源科技有限责任公司
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