CN108148000B - Preparation method of 5, 5-dimethylhydantoin - Google Patents
Preparation method of 5, 5-dimethylhydantoin Download PDFInfo
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- CN108148000B CN108148000B CN201810228468.4A CN201810228468A CN108148000B CN 108148000 B CN108148000 B CN 108148000B CN 201810228468 A CN201810228468 A CN 201810228468A CN 108148000 B CN108148000 B CN 108148000B
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/66—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D233/72—Two oxygen atoms, e.g. hydantoin
- C07D233/74—Two oxygen atoms, e.g. hydantoin with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to other ring members
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Abstract
The invention relates to a preparation method of 5,5 dimethyl hydantoin, which comprises the following steps of 1, weighing 30-70 parts of water, 15-50 parts of ammonium bicarbonate and 10-40 parts of acetone cyanohydrin; reacting in a first reaction kettle at the temperature of 20-50 ℃ to obtain a crude product of 5,5 dimethyl hydantoin; 2 weighing 30-80 parts by weight of 5, 5-dimethylhydantoin crude product and 30-80 parts by weight of water, adding the mixture into a second reaction kettle, heating to 40-60 ℃, adding 0.1-0.5 part by weight of activated carbon into the second reaction kettle, heating to 80-95 ℃, preserving heat for 30 minutes, performing secondary filtration on the material, pressing the material into a third reaction kettle, keeping the temperature at 65-85 ℃, preserving heat for 10 minutes, filtering, and cooling in a crystallization kettle; 3, drying the materials in a centrifuge. The 5, 5-dimethyl hydantoin prepared by the invention has high purity and low impurity content.
Description
Technical Field
The invention relates to a preparation method of 5, 5-dimethylhydantoin.
Background
5, 5-dimethylhydantoin, also known as 5, 5-dimethylhydantoin (hereinafter DMH). DMH is an important organic synthesis intermediate with wide application range, and is a heterocyclic compound with certain rigid framework. A series of valuable derivatives can be prepared by substitution reactions. Such as: dibromohydantoin, dichlorohydantoin and the like are widely used in the production fields of organic synthesis, medicines, plastics, foods, cosmetics, pesticides and the like. Among them, medical 5,5 dimethylhydantoin has better requirements for purity, impurity content and the like, so that development of a preparation method of 5,5 dimethylhydantoin with high purity and low impurity is needed.
Disclosure of Invention
The invention aims to provide a preparation method of 5,5 dimethyl hydantoin, and the prepared 5,5 dimethyl hydantoin has high purity and low impurity content.
In order to achieve the purpose, the invention comprises the following steps of (1) respectively weighing 30-70 parts of water, 15-50 parts of ammonium bicarbonate and 10-40 parts of acetone cyanohydrin; firstly, putting the weighed water and ammonium bicarbonate into a first reaction kettle, stirring until the water and the ammonium bicarbonate are completely dissolved, then adding the weighed acetone cyanohydrin, reacting for 4-10 hours at the temperature of 20-50 ℃ and under the pressure of 0.1MPa in the first reaction kettle, then cooling the materials in the first reaction kettle to the temperature of 20-40 ℃, and cooling for 6-10 hours to obtain a 5, 5-dimethyl hydantoin crude product;
(2) weighing 30-80 parts by weight of the crude 5, 5-dimethylhydantoin obtained in the step (1) and 30-80 parts by weight of water, adding the mixture into a second reaction kettle, stirring and dissolving, heating the material heated in the second reaction kettle to 40-60 ℃, adding 0.1-0.5 part by weight of activated carbon into the second reaction kettle, continuing to heat the second reaction kettle, decoloring and preserving heat for 30 minutes when the temperature of the material in the second reaction kettle reaches 80-95 ℃, then sequentially performing secondary filtration on the material in the second reaction kettle through a titanium rod microporous filter and a bag type microporous filter, then pressing the material into a third reaction kettle under the pressure of 0.1-0.4MPa, keeping the temperature of the material in the third reaction kettle at 65-85 ℃, preserving heat for 10 minutes, sequentially pressing a cationic resin column and an anionic resin column under the pressure of 0.1-0.3MPa for filtration, filtering, pressing the filtrate into a crystallization kettle under the pressure of 0.1-0.3MPa, and cooling at the ambient temperature lower than 30 ℃ for recrystallization;
(3) when the temperature of the materials in the crystallization kettle is reduced to 25-35 ℃, the materials in the crystallization kettle are subjected to liquid removal in a centrifuge at the rotating speed of 950 revolutions per minute, and the centrifuged materials are dried at the drying temperature of 110-150 ℃ for 4 hours.
Further, the weight parts of water in the step (1) are 50-70 parts, the weight parts of ammonium bicarbonate is 25-35 parts, and the weight parts of acetone cyanohydrin is 25-35 parts.
Further, the total volume of the water and the ammonium bicarbonate in the step (1) accounts for 50-80% of the total volume of the first reaction kettle.
Further, in the step (2), the total volume of the 5, 5-dimethylhydantoin crude product and the water accounts for 70-90% of the total volume of the second reaction kettle.
Further, the stirring rate in the step (1) and the step (2) is 50 to 150 revolutions per minute.
Further, in the step (2), the titanium rod microporous filter is T-17 type, the external dimension is 620mm multiplied by 850mm, the theoretical aperture is 0.1 um-30 um, and the theoretical flow is 5.0-7.0T/h;
the model of the microporous bag filter is DL-5P2S, the number of filter bags is 5, the filter area is 2.5 square meters, the maximum flow rate is 175 cubic meters per hour, and the working pressure is 0.5 MPa.
Furthermore, in the step (2), the weight parts of the 5, 5-dimethyl hydantoin crude product, the water and the activated carbon are respectively 40-60 parts, 40-60 parts and 0.2-0.3 part.
Further, in the step (2), the second reaction kettle is a jacketed enamel kettle, the 5, 5-dimethyl hydantoin crude product obtained in the step (1) and water are weighed and added into the second reaction kettle together for stirring and dissolving, then steam is introduced into a jacket of the enamel kettle, the material in the second reaction kettle is heated to 85-95 ℃, the flow of the introduced steam is 0.2 ton/h, and the steam temperature is 140-.
Further, in the step (2), the materials in the third reaction kettle pass through the cationic resin column to remove sodium ions, potassium ions, iron ions, calcium ions and magnesium ions.
Further, in the step (2), the materials in the third reaction kettle pass through the anion resin column to remove sulfate ions, chloride ions and bromide ions in the materials.
The invention has the following positive effects:
the preparation method is simple, and the prepared product has high content of 5, 5-dimethylhydantoin, and low content of sodium ions, iron ions, calcium ions, magnesium ions, sulfate ions, chloride ions, bromide ions and heavy metals (calculated as Pb), and can be used as a medical intermediate.
Detailed Description
The following describes embodiments of the present invention in further detail.
Example 1
(1) Respectively weighing 30 parts of water, 25 parts of ammonium bicarbonate and 35 parts of acetone cyanohydrin; firstly, putting the weighed water and ammonium bicarbonate into a first reaction kettle, stirring until the water and the ammonium bicarbonate are completely dissolved, wherein the stirring speed is 50 revolutions per minute, then adding the weighed acetone cyanohydrin, reacting in the first reaction kettle at 40 ℃ and 0.1MPa for 8 hours, and then cooling the materials in the first reaction kettle to 35 ℃ for 6 hours to obtain a 5,5 dimethyl hydantoin crude product; and (2) the total volume of the water and the ammonium bicarbonate in the step (1) accounts for 50% of the total volume of the first reaction kettle.
(2) Weighing 50 parts by weight of the 5, 5-dimethylhydantoin crude product obtained in the step (1) and 40 parts by weight of water, adding the mixture into a second reaction kettle, stirring and dissolving, heating the material in the second reaction kettle to 40 ℃, adding 0.3 part by weight of activated carbon into the second reaction kettle, continuously heating the second reaction kettle, decoloring and preserving heat for 30 minutes when the temperature of the material in the second reaction kettle reaches 80 ℃, then sequentially performing secondary filtration on the material in the second reaction kettle through a titanium rod microporous filter and a microporous bag filter, then pressing the material into a third reaction kettle under the pressure of 0.1MPa, keeping the temperature of the material in the third reaction kettle at 70 ℃, preserving heat for 10 minutes, sequentially pressing the material into a cation resin column and an anion resin column under the pressure of 0.3MPa for filtration, pressing the filtrate into a crystallization kettle under the pressure of 0.1MPa after filtration, and cooling at an ambient temperature of less than 30 ℃ for recrystallization; in the step (2), the total volume of the 5, 5-dimethyl hydantoin crude product and the water accounts for 70% of the total volume of the second reaction kettle. In the step (2), the titanium rod microporous filter is T-17 type, the external dimension is 620mm multiplied by 850mm, the theoretical aperture is 0.1 um-30 um, and the theoretical flow is 5.0-7.0T/h; the model of the microporous bag filter is DL-5P2S, the number of filter bags is 5, the filter area is 2.5 square meters, the maximum flow rate is 175 cubic meters per hour, and the working pressure is 0.5 MPa.
The cation resin column is 001 × 4,001 × 7 or other cation resin, and the anion resin column
The anion resin is 201 × 4,201 × 7.
(3) When the temperature of the materials in the crystallization kettle is reduced to 35 ℃, the materials in the crystallization kettle are subjected to liquid removal in a centrifuge at the rotating speed of 950 revolutions per minute, and the centrifuged materials are dried at the drying temperature of 150 ℃ for 4 hours.
Example 2
(1) Respectively weighing 70 parts of water, 50 parts of ammonium bicarbonate and 40 parts of acetone cyanohydrin; firstly, putting the weighed water and ammonium bicarbonate into a first reaction kettle, stirring until the water and the ammonium bicarbonate are completely dissolved, wherein the stirring speed is 150 revolutions per minute, then adding the weighed acetone cyanohydrin, reacting in the first reaction kettle at 20 ℃ and 0.1MPa for 10 hours, then cooling the materials in the first reaction kettle to 40 ℃, and cooling for 8 hours to obtain a 5, 5-dimethyl hydantoin crude product; and (2) the total volume of the water and the ammonium bicarbonate in the step (1) accounts for 80% of the total volume of the first reaction kettle.
(2) Weighing 60 parts by weight of the 5, 5-dimethylhydantoin crude product obtained in the step (1) and 60 parts by weight of water, adding the mixture into a second reaction kettle, stirring and dissolving, heating the material in the second reaction kettle to 50 ℃, adding 0.5 part by weight of activated carbon into the second reaction kettle, continuously heating the second reaction kettle, decoloring and preserving heat for 30 minutes when the temperature of the material in the second reaction kettle reaches 95 ℃, then sequentially performing secondary filtration on the material in the second reaction kettle through a titanium rod microporous filter and a microporous bag filter, then pressing the material into a third reaction kettle under the pressure of 0.4MPa, keeping the temperature of the material in the third reaction kettle at 65 ℃, preserving heat for 10 minutes, sequentially pressing the material into a cation resin column and an anion resin column under the pressure of 0.2MPa for filtration, pressing the filtrate into a crystallization kettle under the pressure of 0.3MPa after filtration, and cooling at an ambient temperature of less than 30 ℃ for recrystallization; in the step (2), the total volume of the 5, 5-dimethyl hydantoin crude product and the water accounts for 90% of the total volume of the second reaction kettle. In the step (2), the titanium rod microporous filter is T-17 type, the external dimension is 620mm multiplied by 850mm, the theoretical aperture is 0.1 um-30 um, and the theoretical flow is 5.0-7.0T/h; the model of the microporous bag filter is DL-5P2S, the number of filter bags is 5, the filter area is 2.5 square meters, the maximum flow rate is 175 cubic meters per hour, and the working pressure is 0.5 MPa.
The cation resin column is 001 × 4,001 × 7 or other cation resin, and the anion resin column
The anion resin is 201 × 4,201 × 7.
(3) When the temperature of the materials in the crystallization kettle is reduced to 30 ℃, the materials in the crystallization kettle are subjected to liquid removal in a centrifuge at the rotating speed of 950 revolutions per minute, and the centrifuged materials are dried at the drying temperature of 110 ℃ for 4 hours.
Example 3
(1) Respectively weighing 70 parts of water, 35 parts of ammonium bicarbonate and 25 parts of acetone cyanohydrin; firstly, putting the weighed water and ammonium bicarbonate into a first reaction kettle, stirring until the water and the ammonium bicarbonate are completely dissolved, wherein the stirring speed is 100 revolutions per minute, then adding the weighed acetone cyanohydrin, reacting in the first reaction kettle at 50 ℃ and 0.1MPa for 4 hours, then cooling the materials in the first reaction kettle to 20 ℃, and cooling for 10 hours to obtain a 5, 5-dimethyl hydantoin crude product; the total volume of the water and the ammonium bicarbonate in the step (1) accounts for 70% of the total volume of the first reaction kettle.
(2) Weighing 80 parts by weight of the 5, 5-dimethylhydantoin crude product obtained in the step (1) and 80 parts by weight of water, adding the mixture into a second reaction kettle, stirring and dissolving, heating the material in the second reaction kettle to 60 ℃, adding 0.2 part by weight of activated carbon into the second reaction kettle, continuously heating the second reaction kettle, decoloring and preserving heat for 30 minutes when the temperature of the material in the second reaction kettle reaches 90 ℃, then sequentially performing secondary filtration on the material in the second reaction kettle through a titanium rod microporous filter and a microporous bag filter, then pressing the material into a third reaction kettle under the pressure of 0.3MPa, keeping the temperature of the material in the third reaction kettle at 85 ℃, preserving heat for 10 minutes, sequentially pressing the material into a cation resin column and an anion resin column under the pressure of 0.1MPa for filtration, pressing the filtrate into a crystallization kettle under the pressure of 0.2MPa after filtration, and cooling at an ambient temperature of less than 30 ℃ for recrystallization; in the step (2), the total volume of the 5, 5-dimethyl hydantoin crude product and the water accounts for 80% of the total volume of the second reaction kettle. In the step (2), the titanium rod microporous filter is T-17 type, the external dimension is 620mm multiplied by 850mm, the theoretical aperture is 0.1 um-30 um, and the theoretical flow is 5.0-7.0T/h; the model of the microporous bag filter is DL-5P2S, the number of filter bags is 5, the filter area is 2.5 square meters, the maximum flow rate is 175 cubic meters per hour, and the working pressure is 0.5 MPa.
The cation resin column is 001 × 4,001 × 7 or other cation resin, and the anion resin column
The anion resin is 201 × 4,201 × 7.
(3) When the temperature of the materials in the crystallization kettle is reduced to 25 ℃, the materials in the crystallization kettle are dried in a centrifuge at the rotation speed of 950 revolutions per minute, and the dried materials are dried at the drying temperature of 130 ℃ for 4 hours.
Example 4
(1) Respectively weighing 50 parts of water, 15 parts of ammonium bicarbonate and 10 parts of acetone cyanohydrin; firstly, putting the weighed water and ammonium bicarbonate into a first reaction kettle, stirring until the water and the ammonium bicarbonate are completely dissolved, wherein the stirring speed is 120 r/min, then adding the weighed acetone cyanohydrin, reacting in the first reaction kettle at 35 ℃ and 0.1MPa for 5 hours, then cooling the materials in the first reaction kettle to 28 ℃, and cooling for 7 hours to obtain a 5, 5-dimethyl hydantoin crude product; and (2) the total volume of the water and the ammonium bicarbonate in the step (1) accounts for 60% of the total volume of the first reaction kettle.
(2) Weighing 30 parts by weight of the 5, 5-dimethylhydantoin crude product obtained in the step (1) and 30 parts by weight of water, adding the mixture into a second reaction kettle, stirring and dissolving, heating the material in the second reaction kettle to 48 ℃, adding 0.1 part by weight of activated carbon into the second reaction kettle, continuously heating the second reaction kettle, decoloring and preserving heat for 30 minutes when the temperature of the material in the second reaction kettle reaches 85 ℃, then sequentially passing the material in the second reaction kettle through a titanium rod microporous filter and a microporous bag filter for secondary filtration, then pressing the material into a third reaction kettle under the pressure of 0.25MPa, keeping the temperature of the material in the third reaction kettle at 75 ℃, preserving heat for 10 minutes, sequentially pressing the material into a cation resin column and an anion resin column under the pressure of 0.25MPa for filtration, pressing the filtrate into a crystallization kettle under the pressure of 0.25MPa after filtration, and cooling at an ambient temperature of less than 30 ℃ for recrystallization; in the step (2), the total volume of the 5, 5-dimethyl hydantoin crude product and the water accounts for 85% of the total volume of the second reaction kettle. In the step (2), the titanium rod microporous filter is T-17 type, the external dimension is 620mm multiplied by 850mm, the theoretical aperture is 0.1 um-30 um, and the theoretical flow is 5.0-7.0T/h; the model of the microporous bag filter is DL-5P2S, the number of filter bags is 5, the filter area is 2.5 square meters, the maximum flow rate is 175 cubic meters per hour, and the working pressure is 0.5 MPa.
The cation resin column is 001 × 4,001 × 7 or other cation resin, and the anion resin column
The anion resin is 201 × 4,201 × 7.
(3) When the temperature of the materials in the crystallization kettle is reduced to 25 ℃, the materials in the crystallization kettle are subjected to liquid removal in a centrifuge at the rotating speed of 950 revolutions per minute, the centrifuged materials are dried at the drying temperature of 135 ℃ for 4 hours.
Example 5
(1) Weighing 65 parts of water, 28 parts of ammonium bicarbonate and 31 parts of acetone cyanohydrin; firstly, putting the weighed water and ammonium bicarbonate into a first reaction kettle, stirring until the water and the ammonium bicarbonate are completely dissolved, wherein the stirring speed is 120 r/min, then adding the weighed acetone cyanohydrin, reacting in the first reaction kettle at 42 ℃ and 0.1MPa for 7 hours, then cooling the materials in the first reaction kettle to 33 ℃, and cooling for 8 hours to obtain a 5, 5-dimethyl hydantoin crude product; and (2) the total volume of the water and the ammonium bicarbonate in the step (1) accounts for 65% of the total volume of the first reaction kettle.
(2) Weighing 40 parts by weight of the 5, 5-dimethylhydantoin crude product obtained in the step (1) and 55 parts by weight of water, adding the weighed 5, 5-dimethylhydantoin crude product and 55 parts by weight of water into a second reaction kettle, stirring and dissolving, heating the material in the second reaction kettle to 52 ℃, adding 0.25 part by weight of activated carbon into the second reaction kettle, continuously heating the second reaction kettle, decoloring and preserving heat for 30 minutes when the temperature of the material in the second reaction kettle reaches 88 ℃, then sequentially passing the material in the second reaction kettle through a titanium rod microporous filter and a microporous bag filter for secondary filtration, then pressing the material into a third reaction kettle under the pressure of 0.28MPa, keeping the temperature of the material in the third reaction kettle at 72 ℃, preserving heat for 10 minutes, sequentially pressing the material into a cation resin column and an anion resin column under the pressure of 0.25MPa for filtration, pressing the filtrate into a crystallization kettle under the pressure of 0.25MPa after filtration, and cooling at an ambient temperature of less than 30 ℃ for recrystallization; in the step (2), the total volume of the 5, 5-dimethyl hydantoin crude product and the water accounts for 80% of the total volume of the second reaction kettle. In the step (2), the titanium rod microporous filter is T-17 type, the external dimension is 620mm multiplied by 850mm, the theoretical aperture is 0.1 um-30 um, and the theoretical flow is 5.0-7.0T/h; the model of the microporous bag filter is DL-5P2S, the number of filter bags is 5, the filter area is 2.5 square meters, the maximum flow rate is 175 cubic meters per hour, and the working pressure is 0.5 MPa.
The cation resin column is 001 × 4,001 × 7 or other cation resin, and the anion resin column
The anion resin is 201 × 4,201 × 7.
(3) When the temperature of the materials in the crystallization kettle is reduced to 29 ℃, the materials in the crystallization kettle are subjected to liquid removal in a centrifuge at the rotating speed of 950 rpm, and the centrifuged materials are dried at the drying temperature of 128 ℃ for 4 hours.
The content of 5, 5-dimethylhydantoin finally obtained in example 5 is tested, and the content of 5, 5-dimethylhydantoin is detected by a high performance liquid chromatograph; the melting point is detected by using a WRR melting point instrument; drying the sample for 2 hours at 80 ℃ under vacuum to measure the drying weight loss; detecting the chroma by a platinum-cobalt chroma meter; detecting metal ions such as sodium, iron, calcium, magnesium, lead and the like by using an inductively coupled plasma emission spectrometer according to JY/T015-1996; sulfate ions, chloride ions and bromide ions are detected by an ion spectrometer according to JY/T020-1996, and the results are as follows:
99.96 percent of 5, 5-dimethyl hydantoin, 178.0 percent of initial melting point, 0.05 percent of drying weight loss, 4APHA chroma, 0.5mg/kg of sodium ions, 1mg/kg of iron ions, 2mg/kg of calcium ions, 0.2mg/kg of magnesium ions, 1mg/kg of sulfate ions, 5mg/kg of chloride ions, 0.1mg/kg of bromide ions and 6mg/kg of heavy metals (calculated as Pb). Therefore, the 5, 5-dimethylhydantoin prepared by the preparation method disclosed by the invention has high purity and low impurity content and can be used as a medical intermediate.
The detection result of each technical index of the common commercial product 5,5 dimethyl hydantoin is as follows:
99.0 percent of 5, 5-dimethyl hydantoin, an initial melting point of 175.8.0 ℃, a drying weight loss of 0.5 percent, a chromaticity of 25APHA, 25mg/kg of sodium ions, 21mg/kg of iron ions, 41mg/kg of calcium ions, 15mg/kg of magnesium ions, 29mg/kg of sulfate ions, 48mg/kg of chloride ions, 26mg/kg of bromide ions and 35mg/kg of heavy metals (calculated as Pb).
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of 5,5 dimethyl hydantoin is characterized in that: comprises the following steps of (a) carrying out,
(1) respectively weighing 30-70 parts of water, 15-50 parts of ammonium bicarbonate and 10-40 parts of acetone cyanohydrin; firstly, putting the weighed water and ammonium bicarbonate into a first reaction kettle, stirring until the water and the ammonium bicarbonate are completely dissolved, then adding the weighed acetone cyanohydrin, reacting for 4-10 hours at the temperature of 20-50 ℃ and under the pressure of 0.1MPa in the first reaction kettle, then cooling the materials in the first reaction kettle to the temperature of 20-40 ℃, and cooling for 6-10 hours to obtain a 5, 5-dimethyl hydantoin crude product;
(2) weighing 30-80 parts by weight of the crude 5, 5-dimethylhydantoin obtained in the step (1) and 30-80 parts by weight of water, adding the mixture into a second reaction kettle, stirring and dissolving, heating the material heated in the second reaction kettle to 40-60 ℃, adding 0.1-0.5 part by weight of activated carbon into the second reaction kettle, continuing to heat the second reaction kettle, decoloring and preserving heat for 30 minutes when the temperature of the material in the second reaction kettle reaches 80-95 ℃, then sequentially passing the material in the second reaction kettle through a titanium rod microporous filter and a bag type microporous filter for secondary filtration, then pressing the material into a third reaction kettle under the pressure of 0.1-0.4MPa, keeping the temperature of the material in the third reaction kettle at 65-85 ℃, preserving heat for 10 minutes, sequentially pressing the material into a cation resin column and an anion resin column under the pressure of 0.1-0.3MPa for filtration, filtering, pressing the filtrate into a crystallization kettle under the pressure of 0.1-0.3MPa, and cooling at the ambient temperature lower than 30 ℃ for recrystallization;
(3) when the temperature of the materials in the crystallization kettle is reduced to 25-35 ℃, the materials in the crystallization kettle are subjected to liquid removal in a centrifuge at the rotating speed of 950 revolutions per minute, and the centrifuged materials are dried at the drying temperature of 110-150 ℃ for 4 hours.
2. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: 50-70 parts of water, 25-35 parts of ammonium bicarbonate and 25-35 parts of acetone cyanohydrin in the step (1).
3. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: and (2) the total volume of the water and the ammonium bicarbonate in the step (1) accounts for 50-80% of the total volume of the first reaction kettle.
4. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: in the step (2), the total volume of the 5, 5-dimethyl hydantoin crude product and the water accounts for 70-90% of the total volume of the second reaction kettle.
5. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: the stirring speed in the step (1) and the step (2) is 50-150 revolutions per minute.
6. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: in the step (2), the titanium rod microporous filter is T-17 type, the external dimension is 620mm multiplied by 850mm, the theoretical aperture is 0.1 um-30 um, and the theoretical flow is 5.0-7.0T/h;
the model of the microporous bag filter is DL-5P2S, the number of filter bags is 5, the filter area is 2.5 square meters, the maximum flow rate is 175 cubic meters per hour, and the working pressure is 0.5 MPa.
7. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: in the step (2), the weight parts of the 5, 5-dimethyl hydantoin crude product, the water and the activated carbon are respectively 40-60 parts, 40-60 parts and 0.2-0.3 part.
8. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: in the step (2), the second reaction kettle is a jacketed enamel kettle, the 5, 5-dimethyl hydantoin crude product obtained in the step (1) and water are weighed and added into the second reaction kettle together for stirring and dissolving, then steam is introduced into a jacket of the enamel kettle, the material in the second reaction kettle is heated to 85-95 ℃, the flow of the introduced steam is 0.2 ton/h, and the steam temperature is 140-.
9. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: in the step (2), the materials in the third reaction kettle pass through the cationic resin column to remove sodium ions, potassium ions, iron ions, calcium ions and magnesium ions.
10. The method for preparing 5,5 dimethylhydantoin according to claim 1, wherein: in the step (2), the materials in the third reaction kettle pass through the anion resin column to remove sulfate ions, chloride ions and bromide ions in the materials.
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| CN100369901C (en) * | 2006-01-23 | 2008-02-20 | 周新基 | Method for preparing 5,5-dimethylhydantion |
| CN102002000B (en) * | 2010-11-18 | 2012-07-25 | 祝莉宁 | Method for producing 5,5-dimethyl hydantoin |
| CN103333115B (en) * | 2013-07-15 | 2015-01-21 | 河北鑫淘源环保科技有限公司 | Production method of bromo-3-chloro-5,5-dimethylhydantoin (BCDMH) serving as chemical intermediate |
| CN104557721B (en) * | 2014-12-30 | 2017-12-15 | 沈阳化工研究院有限公司 | A kind of method for producing 5,5 DMHs |
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