On the one hand, the invention provides a purification method of 1,1, 3-trichloroacetone, wherein the method comprises the following steps

Flash:

(1) Crude 1,1, 3-trichloroacetone mixed with water;

(2) Recrystallization of the upper solution after standing; As well as

(3) the recrystallized solid crystals are filtered out and washed with water;

Wherein, in Step (1), the weight ratio of the said crude 1,1, 3-trichloroacetone to the amount of water is 1 0.1-2).

Preferably, in Step (1), the weight ratio of the 1,1, 3-trichloroacetone crude product to the amount of water can be 1:

(0.4-0.6), further optimized as 1:0.5; In the invention, the dosage of 1,1, 3-trichloroacetone crude product and water is controlled in the above

The range of high purity 1,1, 3-trichloroacetone can be obtained.

According to the present invention, in step (1), the 1,1, 3-trichloroacetone crude product and water can be prepared at a temperature of 10-50℃

Mix for 10-30 minutes under the conditions, and then let stand for 10-30 minutes; Preferably, in Step (1), said 1,1, 3-trichloropropyl

The crude ketone was mixed with water at a temperature of 30-35℃ for 25-30 minutes, and then stood for 10-15 minutes; In the present invention

, using 1,1, 3-trichloroacetone crude as raw material, in the reaction kettle, mixed with water, stirred at a certain temperature after standing

Delamination. After delamination, the lower oil layer is removed, mainly by removing high chlorine impurities and leaving the upper solution for later use.

According to the invention, in step (1), the crude 1,1, 3-trichloroacetone is mixed with water and can also be stirred

Conditions, in which there is no specific limitation on the stirring conditions and equipment, as long as the 1,1, 3-trichloroacetone can be coarse

The product can be evenly mixed with water. Preferably, the mixing rate is 100-300r/min.

In the present invention, the water is preferably deionized water.

According to the invention, in step (2), the recrystallization conditions may be: temperature from 0 to 35℃, time from 0.5 -

10 hours, preferably, the recrystallization is carried out at a stirring rate of 50-300 RPM; Preferably, the reknot

Water is also added in the crystallization process, wherein the water is added at a rate of 200-600 ml/min; Under these conditions, recrystallization efficiency

Fruit is good.

[0034] Further optimally, the recrystallization conditions are: a temperature of 10-15℃, a time of 2-3 hours, and the recrystallization conditions

The crystal is stirred at a rate of 100-200 RPM and the water is added at a rate of 300-500 ml/min.

Under these conditions, the recrystallization effect is better.

In the present invention, the recrystallization temperature described in step (2) is lower than that of 1,1, 3-trichloroacetone in step (1)

The temperature at which the product is mixed with water.

According to the invention, in Step (3), the reaction mixture after Step (2) can be filtered out by closed pressure, or can be

Solid crystals are obtained by pressing directly through the sieve plate at the bottom of the reactor. In the present invention, air and/or nitrogen are preferably used

Pressure filtration, it is better to use nitrogen for pressure filtration, and the pressure can be 0.1-0.2MPa, preferably 0.12 -

0. 18 mpa.

According to the invention, the precipitated crystal after pressure filtration is washed with water, wherein the said water is washed

There is no specific limit, for example, you can choose 1-2kg of water spray washing under the condition of the temperature of 2-25℃, and spray

There is no specific speed limit.

According to the invention, the purity of the 1,1, 3-trichloroacetone crude product may be 50-65 % by weight.

Pages 3/6 of instruction

5

CN 109516908 A

5

The present invention, on the other hand, also provides a folic acid which is prepared by any of the methods described above

An aqueous solution of 1,1, 3-trichloroacetone is directly used to prepare folic acid.

The operation of the purification method of the invention, such as stratified extraction, crystallization filtration and so on, can be carried out in a closed system

Environment-friendly, and greatly reduce the generation of waste water, no waste organic solvents and organic waste gas; In addition, the purification method

No organic solvents are introduced, and the high chlorine impurities are removed during the purification process, so there is no quality risk to the quality of folic acid

The method uses water as the crystallization solvent, and the purified aqueous solution of 1,1, 3-trichloroacetone is directly used for the production of folic acid

The total yield of folic acid can be increased by 5 % by weight, and the purity is above 99.2 % by weight, which can obtain high quality

Of folic acid.

The invention is described in detail by means of embodiments below.

[0042] In the following embodiments and proportions, unless otherwise specified, the materials used are available through commercial purchase, unless otherwise specified

The method used is the conventional method in this field.

The gas chromatography model was GC-2014, purchased from Shimadzu Company.

The 1,1, 3-trichloroacetone prepared by the purification method of the present invention [0047] is purified in a 50-litre reactor equipped with a filter sieve plate at the bottom [0048] First, the purity of 1,1 is 65 % by weight , 3-trichloroacetone 20Kg and water 10Kg in the reaction kettle mixed in 24 stirring for 12 minutes, where the stirring rate is 200r/min, in the stirring process to add water, the water at a rate of 300 ml /min, and then the mixture stood for 10 minutes, separated from the lower oil layer, remove high chlorine impurities; Secondly, the temperature of the layered upper solution was lowered to 5 and stirred for 2 hours at a stirring rate of 100r/min. Then, the solid crystal was obtained directly through the sieve plate at the bottom of the reaction kettle by nitrogen pressure filtration at a pressure of 0.1 MPa, and then sprayed and washed with 2 kg cold water. The wet weight of 1,1, 3-trichloroacetone was 9.8 kg, and the chromatographic pure (GC) was 96.8 wt % [0051] The operation involved in this purification method, such as static stratification, removal of high chlorine impurities, crystallization, filtration and water washing, can be carried out in a closed body system, which is environmentally friendly, and greatly reduces the generation of waste water and does not produce waste organic solvent and organic waste gas [0052]. In addition, because the purification method without introducing organic solvent, and high chlorine to remove impurities in the purification process, there is no quality risk on quality of folic acid, but also by the implementation example of the preparation of 1, 1, 3 – folic acid cross-linked with acetone water dissolved directly used in production, makes folic acid to improve overall yield 5 weight %, the purity of 99 5 weight % Example 2 [0054] This embodiment states that 1,1, 3-trichloroacetone prepared by the purification method of the present invention [0055] is purified in a 50-litre reactor equipped with a filter sieve plate at the bottom [0056] First,1,1 with a purity of 50% , 3-trichloroacetone 20Kg and water 4Kg mixed in the reactor, stirring for 15 minutes at 45, the stirring rate of 300r/min, in the stirring process to add water, the water at a rate of 300 ml /min, and then the mixture stood for 15 minutes, separated from the lower oil layer, remove high chlorine impurities; Secondly, the temperature of the upper layer solution after stratification was lowered to 20, and the stirring rate was 200r/min for 0.5 h. Then, the solid crystal was obtained directly through the sieve plate at the bottom of the reactor by nitrogen pressure filtration at the pressure of 0. 2MPa. Then, the solid crystal was sprayed and washed with 1Kg of 25 cold water, and the wet weight of 1,1, 3-trichloroacetone was 8.2kg by the method of reduction The purification method involved in the static stratification removal of high chlorine impurities, crystallization, filtration and water washing operations can be carried out in A closed body system, the working environment is friendly, and greatly reduce the generation of waste water, no waste organic solvent and organic waste gas [0060] In addition, since the method does not introduce organic solvents and removes high chlorine impurities during the purification process, there is no quality risk to the quality of folic acid, and the 1,1, 3-trichloroacetone prepared by Example 2 is dissolved in water and directly used in the production of folic acid, increasing the total yield of folic acid by 4.9% by weight and achieving a purity of 99 This embodiment states that the 1,1, 3-trichloroacetone prepared by the purification method of the present invention [0063] is purified in a 50-litre reactor fitted with a filter sieve plate at the bottom [0064] First,1,1 with a purity of 60% , 3-trichloroacetone 20Kg mixed with water 40Kg in the reaction kettle, stirring for 30 minutes at 15, the stirring rate of 100r/min, in the stirring process to add water, the water at a rate of 500 ml /min, and then the mixture stood for 30 minutes, separated from the lower oil layer, remove high chlorine impurities; Secondly, the temperature of the upper layer solution after stratification was lowered to 10, and the stirring rate was 100r/min for 10 hours. Then, the solid crystal was obtained directly through the sieve plate at the bottom of the reactor by nitrogen pressure filtration at the pressure of 0.2MPa, and then sprayed and washed with 1Kg of 5 cold water. The wet weight of 1,1, 3-trichloroacetone was 6.9kg, and the chromatographic pure (GC) was 98.3% by weight [0067] The operation involved in this purification method, such as static stratification, removal of high chlorine impurities, crystallization, filtration and water washing, can be carried out in a closed body system, which has a friendly working environment, and greatly reduces the generation of waste water and does not produce waste organic solvent and organic waste gas [0068]. In addition, because the purification method without introducing organic solvent, and high chlorine to remove impurities in the purification process, there is no quality risk on quality of folic acid, and will be for example 3 preparation of 1, 1, 3 – cross-linked with acetone, water to dissolve, directly used in production of folic acid, makes folic acid to improve overall yield 5. 3 weight %, the purity of 99. 2 weight % For proportion 1 [0070] purified 1,1, 3-trichloroacetone according to the method of embodiment 1, except that in step (1), water is not used, Instead, organic solvents were used. As a result, the prepared 1,1, 3-trichloroacetone was dissolved in water and directly used in the production of folic acid. The total yield of folic acid was only increased by 2 % by weight and the purity was 95 % by weight. In addition, due to the introduction of organic solvents in this purification method, there is a quality risk to the quality of folic acid [0071] in proportion 2 [0072]. 1,1, 3-trichloroacetone is purified according to the method in Example 1. The difference is that in Step (1), the amount of water is 50Kg, resulting in a significant increase in the generation of wastewater and a decrease of 1 The yield of 1,1, 3-trichloroacetone crystals was dissolved in water and directly used in the production of folic acid, so that the total yield of folic acid was only increased by 5.6% by weight and the purity was 99.6% by weight [0073] against the ratio of 3 [0074]. 1,1 was purified by the method of Example 1 , 3-trichloroacetone, the difference is that in step (1), the high chlorine heteroplastid is not removed, the result of the preparation of 1,1, 3-trichloroacetone contains a large number of chlorinated compounds, the quality of folic acid risk [0075] According to the above example 1-3 and is the result of the scale of 1-3: the purification method involves let stand layered crystal filter to remove high chlorine impurities washing operations such as all but in the airtight system, friendly working environment, and greatly reduced the incidence of waste water, does not produce waste gas, organic solvent and organic In addition, by implementing case 1 the preparation of 1, 1) , 3-trichloroacetone, add in the book 5/6 page 7 CN 109516908 A 7 water solution, directly used in the production of folic acid, make the total yield of folic acid increased 5 % by weight, purity is 99.2 % by weight above; Moreover, because the purification method does not introduce organic solvent, there is no quality risk to the quality of folic acid. Moreover, the purification method uses water as the crystallization solvent, and the purified aqueous solution of 1,1, 3-trichloroacetone is directly used in the production of folic acid, reducing side reactions

Athena  CEO

Whatsapp/wechat:+86 13805212761

MIT –IVY Industry CO.,LTD

ceo@mit-ivy.com

ADD：Jiangsu Province, China