CN102746310B - A kind of be raw material production industry hexamethylenamine with useless paraformaldehyde method - Google Patents
A kind of be raw material production industry hexamethylenamine with useless paraformaldehyde method Download PDFInfo
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- CN102746310B CN102746310B CN201210233327.4A CN201210233327A CN102746310B CN 102746310 B CN102746310 B CN 102746310B CN 201210233327 A CN201210233327 A CN 201210233327A CN 102746310 B CN102746310 B CN 102746310B
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Abstract
The invention discloses a kind of method being raw material production industry hexamethylenamine with useless paraformaldehyde, its method is that the useless paraformaldehyde solid separated out by formaldehyde storage tank reacts generation hexamethylenamine aqueous solution under pressure with ammonia (or gas ammonia), the mol ratio of paraformaldehyde (being converted into formaldehyde) and ammonia is 6:4.1～4.5, then its aqueous solution decolour, filter, be concentrated in vacuo, crystallisation by cooling, centrifugal and dry prepare hexamethylenamine.The pressure of its reaction is 0.15～0.45Mpa, and reaction temperature is 115 DEG C～150 DEG C, and the response time is 4～6 hours, and the response rate of useless paraformaldehyde is up to more than 98%, and the hexamethylenamine content of production is up to 98%, and water-insoluble is excellent.
Description
Technical field
The present invention relates to a kind of industry hexamethylenamine production method, a kind of be raw material production industry hexamethylenamine with useless paraformaldehyde method.
Background technology
Hexamethylenamine chemical name hexamethylenetetramine, has another name called Urotropinum, and outward appearance is white hygroscopic crystalline powder or colourless glossiness diamond crystal body, flammable, and fusing point 263 DEG C i.e. distils as exceeded this fusing point and decomposes, but not melting；It is warming up to when 300 DEG C release Blausure (German), when temperature raises again, then it is decomposed into methane, hydrogen and nitrogen, relative density 1.331(20/4 DEG C), flash-point 250 DEG C, almost odorless, taste is sweet and bitter, water soluble and chloroform, is insoluble in carbon tetrachloride, acetone, benzene and ether, insoluble in petroleum ether, weak acid solution is decomposed into ammonia and formaldehyde.It is mainly used as resin and the firming agent of plastics, the catalyst of aminoplast and foaming agent, the accelerator (Urotropinum) of the vulcanization of rubber, the anti-piping compound etc. of textile.Hexamethylenetetramine is the raw material of organic synthesis, is used for producing chloromycetin, hexamethylenamine insecticide in medical industry.
Industry hexamethylenamine is condensed by industrial formol and ammonia and prepares, its production process is: be placed in reactor by industrial formaldehyde solution, logical ammonia, carries out condensation reaction in alkaline solution, and reaction temperature is maintained at 50～70 DEG C, feed liquid cooled entrance liquid film vacuum evaporator, evaporate under the conditions of 60～80 DEG C so that it is concentration brings up to 38%～42% from 24%, then by reacting liquid filtering, it is dried through vacuum evaporating crystalization, sucking filtration, obtains industrial hexamethylenamine.
In the production and storage of formaldehyde; formaldehyde can occur self-polymeric reaction; generate the paraformaldehyde that molecular size range does not waits; these paraformaldehyde outward appearances are faint yellow granule or powder; it is difficult to be dissolved in water, is the useless paraformaldehyde not having use value, often do the buried process of solid waste; the most not only polluting environment, also resulting in must economic loss.
Summary of the invention
It is an object of the invention to overcome the above-mentioned deficiency of prior art, and a kind of method being raw material production industry hexamethylenamine with useless paraformaldehyde is provided, the useless paraformaldehyde pollution problem to environment can not only be solved, and preferable economic benefit can also be obtained.
The technical scheme is that a kind of method being raw material production industry hexamethylenamine with useless paraformaldehyde, it is that the suspension that the paraformaldehyde water that the paraformaldehyde produced in formaldehyde production or formaldehyde storage tank separate out is configured to solid content 34%～90% adds reactor, the ammonia (or being passed through ammonia) of 15%～25% is added in reactor, paraformaldehyde (being converted into formaldehyde) is 6:4.1～4.2 with the mol ratio of ammonia, reaction pressure is between 0.15～0.45Mpa, reaction temperature is 115 DEG C～150 DEG C, response time is 4～6 hours, the reactant liquor of gained contains after reaction the hexamethylenamine solution of 24%～26%；By reactant liquor insulation under conditions of through decolorizing with activated carbon, filtration, again in vacuum, evaporate under conditions of 60～80 DEG C, the concentration making its hexamethylenamine brings up to 38%～42% from 24%～26%, is then cooled down by concentrated solution, crystallizes centrifugal and be dried prepared hexamethylenamine finished product.
The further technical scheme of the present invention is: the mother solution containing hexamethylenamine of centrifugal gained returns configuration paraformaldehyde suspension.
The paraformaldehyde that the present invention separates out with the paraformaldehyde produced in formaldehyde production or formaldehyde storage tank is as raw material, generation hexamethylenamine is reacted under suitable condition with ammonia (or ammonia), product quality meets GB/T9015-1998 standard, not only solve the pollution problem to environment of the useless paraformaldehyde, and preferable economic benefit can be obtained.
Below in conjunction with detailed description of the invention, the detailed content of the present invention is further described.
Detailed description of the invention
Embodiment one
A kind of be raw material production industry hexamethylenamine with useless paraformaldehyde method, it is paraformaldehyde 1.4 tons (the equivalent 100% formaldehyde amount 1.2 tons paraformaldehyde produced in formaldehyde production or formaldehyde storage tank separated out, after 40Kmol) adding 4000 liters of pressure reaction stills, add 250kg water and be configured to solid content85%Suspension, the ammonia 2380kg of 20% is added again in reactor, paraformaldehyde (being converted into formaldehyde) is 6:4.2 with the mol ratio of ammonia, reaction pressure is between 0.15～0.45Mpa, reaction temperature is 135 DEG C, response time is 5 hours, contains the hexamethylenamine of 24%～26% after reaction in the reactant liquor of gained；By above-mentioned reactant liquor insulation under conditions of through decolorizing with activated carbon, filtration, in vacuum, evaporate under the conditions of 60～80 DEG C, the concentration making its hexamethylenamine brings up to 38%～42% from 24%～26%, then being cooled down by concentrated solution, crystallize, be centrifuged, be dried, prepared content is the hexamethylenamine finished product 850kg of 98.2%.The mother solution containing hexamethylenamine of centrifugal gained returns preparation paraformaldehyde suspension.
Embodiment two
A kind of be raw material production industry hexamethylenamine with useless paraformaldehyde method, it is paraformaldehyde 1.4 tons (the equivalent 100% formaldehyde amount 1.2 tons paraformaldehyde produced in formaldehyde production or formaldehyde storage tank separated out, after 40Kmol) adding 4000 liters of pressure reaction stills, add 2150kg water and be configured to solid content36%Suspension, then in reactor, be passed through ammonia 476kg, paraformaldehyde (being converted into formaldehyde) is 6:4.2 with the mol ratio of ammonia, and reaction pressure is between 0.15～0.45Mpa, and reaction temperature is135DEG C, the response time is5Hour, the reactant liquor of gained contains after reaction the hexamethylenamine of 24%～26%, by above-mentioned reactant liquor insulation under conditions of through decolorizing with activated carbon, filtration, in vacuum, evaporate under the conditions of 60～80 DEG C, the concentration making its hexamethylenamine brings up to 38%～42% from 24%～26%, then being cooled down by concentrated solution, crystallize, be centrifuged, be dried, prepared content is the hexamethylenamine finished product 860kg of 98.4%.The mother solution containing hexamethylenamine of centrifugal gained returns preparation paraformaldehyde suspension.
Embodiment three
A kind of be raw material production industry hexamethylenamine with useless paraformaldehyde method, it is paraformaldehyde 1.4 tons (the equivalent 100% formaldehyde amount 1.2 tons paraformaldehyde produced in formaldehyde production or formaldehyde storage tank separated out, after 40Kmol) adding 4000 liters of pressure reaction stills, add 2150kg water and be configured to solid content36%Suspension, then in reactor, be passed through ammonia 465kg, paraformaldehyde (being converted into formaldehyde) is 6:4.1 with the mol ratio of ammonia, and reaction pressure is between 0.15～0.45Mpa, and reaction temperature is135DEG C, the response time is6Hour, the reactant liquor of gained contains after reaction the hexamethylenamine of 24%～26%；By above-mentioned reactant liquor insulation under conditions of through decolorizing with activated carbon, filtration, in vacuum, evaporate under the conditions of 60～80 DEG C, the concentration making its hexamethylenamine brings up to 38%～42% from 24%～26%, then being cooled down by concentrated solution, crystallize, be centrifuged, be dried, prepared content is the hexamethylenamine finished product 855kg of 98.0%.The mother solution containing hexamethylenamine of centrifugal gained returns preparation paraformaldehyde suspension.
Claims (1)
1. the method producing industry hexamethylenamine with useless paraformaldehyde, is characterized in that Formaldehyde Production mistake
The useless paraformaldehyde water produced in journey is configured to the suspension of solid content 34%～90% and adds reactor,
Adding the ammonia of 15%～20% in reactor, paraformaldehyde is 6:4.1 with the mol ratio of ammonia, reaction pressure
Between 0.15～0.45Mpa, reaction temperature is 115 DEG C～150 DEG C, and the response time is 4～5 hours,
The reactant liquor of gained contains after reaction the hexamethylenamine solution of 24%～26%；By reactant liquor at the bar being incubated
Through decolorizing with activated carbon, filtration under part, then in vacuum, evaporate under conditions of 60～80 DEG C so that it is Wu Luo
The concentration of tropine brings up to 38%～42%, is then cooled down by concentrated solution, crystallizes centrifugal and be dried prepared crow Lip river
Tropine finished product；The mother solution containing hexamethylenamine of centrifugal gained returns configuration paraformaldehyde suspension.
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| CN102746310A CN102746310A (en) | 2012-10-24 |
| CN102746310B true CN102746310B (en) | 2016-09-28 |
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| CN105646166A (en) * | 2015-12-25 | 2016-06-08 | 江苏合泰新材料科技有限公司 | Method for preparing isophthalaldehyde by using paraformaldehyde as oxidant and recycling mother liquor |
| CN113264940A (en) * | 2021-05-18 | 2021-08-17 | 宁夏华业精细化学科技有限公司 | Production process flow of urotropine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1259518A (en) * | 1999-01-05 | 2000-07-12 | 曹官岐 | Prodn. technology of urotropine by ammoniation of formaldehyde |
| RU2198887C1 (en) * | 2002-02-04 | 2003-02-20 | Открытое акционерное общество "МЕТАФРАКС" | Method of synthesis of hexamethylenetetramine (urotropin) |
| CN101497617A (en) * | 2009-03-19 | 2009-08-05 | 杭州天创净水设备有限公司 | Method for producing hexamethylene tetramin by formaldehyde-containing wastewater |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1259518A (en) * | 1999-01-05 | 2000-07-12 | 曹官岐 | Prodn. technology of urotropine by ammoniation of formaldehyde |
| RU2198887C1 (en) * | 2002-02-04 | 2003-02-20 | Открытое акционерное общество "МЕТАФРАКС" | Method of synthesis of hexamethylenetetramine (urotropin) |
| CN101497617A (en) * | 2009-03-19 | 2009-08-05 | 杭州天创净水设备有限公司 | Method for producing hexamethylene tetramin by formaldehyde-containing wastewater |
Non-Patent Citations (2)
| Title |
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| 10kt/a乌洛托品工艺运行小结;于兴辉，等;《小氮肥》;20070515;第35卷(第05期);第19-21页 * |
| 乌洛托品及其生产方法;李广林;《化肥工业》;19970831;第24卷(第04期);第51-53页 * |
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