CN202766441U - Device for preparing 3-methylthiopropionaldehyde through liquid-liquid reaction of methyl mercaptan and acrolein - Google Patents
Device for preparing 3-methylthiopropionaldehyde through liquid-liquid reaction of methyl mercaptan and acrolein Download PDFInfo
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- CN202766441U CN202766441U CN 201220440644 CN201220440644U CN202766441U CN 202766441 U CN202766441 U CN 202766441U CN 201220440644 CN201220440644 CN 201220440644 CN 201220440644 U CN201220440644 U CN 201220440644U CN 202766441 U CN202766441 U CN 202766441U
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Abstract
The utility model discloses a device for preparing 3-methylthiopropionaldehyde through a liquid-liquid reaction of methyl mercaptan and acrolein. The device comprises a reactor, a circulating pump, a mixer I and a mixer II, wherein the material outlet of the reactor is communicated with the material inlet of the circulating pump, the material outlet of the circulating pump is communicated with the material inlet of the mixer I, the material outlet of the mixer I is communicated with the material inlet of the mixer II, the material outlet of the mixer II is communicated with the material inlet of the reactor, a product outlet pipe is arranged on a passage from the circulating pump to the mixer I, and raw material inlet pipes I and II are arranged on the mixers I and II respectively. According to the device, two mixers are added, therefore the methyl mercaptan liquid and the acrolein liquid are fully contacted and evenly mixed, side reactions caused by overhigh local concentration of the methyl mercaptan or the acrolein can be reduced, purity and yield of the product can be improved, and by measurement, the content of the 3-methylthiopropionaldehyde in the liquid reaction product flowing out of the outlet of the reactor reaches above 95%mol, and the yield reaches above 92% mol.
Description
Technical field
The utility model belongs to chemical field, relates to a kind of improved Chemicals preparation facilities.
Background technology
The 3-methylthiopropionaldehyde is the hydroxy analogs of preparation methionine(Met) and methionine(Met), the intermediate commonly used of MHA.Methionine(Met) is the indispensable amino acid in the animal feedstuff compositions.The hydroxy analogs of methionine(Met) is the source of methionine(Met), is widely used as the methionine(Met) fill-in in the animal-feed.
Make thiomethyl alcohol and propenal that Michael reaction occur under catalyst action and can prepare the 3-methylthiopropionaldehyde.One of conventional preparation method introduces liquid thiomethyl alcohol and propylene liquid aldehyde to contain in liquid phase 3-methylthiopropionaldehyde and the reactor as the organic bases of olefin/mercaptan addition reaction catalyst, and reaction is carried out in liquid phase.But the method is in actual production process, owing to being reactive liquid solution, the very fast and exothermic heat of reaction of speed of response is easily because of thiomethyl alcohol or the propenal partial concn is too high and/or local superheating, cause the generation of by product, and then reduce purity and the yield of 3-methylthiopropionaldehyde product.
The utility model content
For the problems referred to above, the purpose of this utility model is to provide a kind of device that is prepared the 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution, can prevent that the too high by product that causes of thiomethyl alcohol or propenal partial concn from generating, and improves purity and the yield of 3-methylthiopropionaldehyde product.
Through research, the utility model provides following technical scheme:
The device that is prepared the 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution comprises reactor, recycle pump, mixing tank I and mixing tank II; The discharge port of described reactor is communicated with the opening for feed of recycle pump, and the discharge port of recycle pump is communicated with the opening for feed of mixing tank I, and the discharge port of mixing tank I is communicated with the opening for feed of mixing tank II, and the discharge port of mixing tank II is communicated with the opening for feed of reactor; Described recycle pump also arranges product discharging pipeline to the path of mixing tank I, material feeding tube road I also is set on the mixing tank I, and material feeding tube road II also is set on the mixing tank II.
Further, described mixing tank I also arranges interchanger to the path of mixing tank II, and the opening for feed of interchanger is communicated with the discharge port of mixing tank I, and the discharge port of interchanger is communicated with the opening for feed of mixing tank II.
The beneficial effects of the utility model are: the utility model is by increasing by 2 mixing tanks in device, make propenal liquid more abundant with contacting of thiomethyl alcohol liquid, mix more even, reduced because of propenal or the too high side reaction that causes of thiomethyl alcohol partial concn, purity and the yield of 3-methylthiopropionaldehyde product have been improved, after measured, from the liquid reacting product that the reactor discharge port flows out, the content of 3-methylthiopropionaldehyde has reached more than the 95%mol, and yield has all reached more than the 92%mol in thiomethyl alcohol or propenal.Further, in said apparatus, increase again 1 interchanger, effectively the control temperature of charge reduces the reactor temperature fluctuation, is beneficial to all reaction systems of relatively stable, equal perseverance of formation temperature, concentration and speed of response, the side reaction that minimizing causes because of the system local superheating, further improve purity and the yield of 3-methylthiopropionaldehyde product, after measured, behind the increase interchanger, the content of 3-methylthiopropionaldehyde can improve approximately 2.5%mol again, and yield can improve approximately 5%mol again in propenal.
Description of drawings
In order to make the purpose of this utility model, technical scheme and advantage clearer, below in conjunction with accompanying drawing the utility model is described in further detail, wherein:
Fig. 1 is for being prepared the apparatus structure schematic diagram of 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution.
Embodiment
Hereinafter with reference to accompanying drawing, preferred embodiment of the present utility model is described in detail.
The apparatus structure schematic diagram for preparing the 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution comprises reactor 1, recycle pump 2, mixing tank I 3, interchanger 4 and mixing tank II 5 as shown in Figure 1; The discharge port of described reactor 1 is communicated with the opening for feed of recycle pump 2, the discharge port of recycle pump 2 is communicated with the opening for feed of mixing tank I 3, the discharge port of mixing tank I 3 is communicated with the opening for feed of interchanger 4, the discharge port of interchanger 4 is communicated with the opening for feed of mixing tank II 5, and the discharge port of mixing tank II 5 is communicated with the opening for feed of reactor 1; Described recycle pump 2 also arranges product discharging pipeline to the path of mixing tank I 3, material feeding tube road I also is set on the mixing tank I 3, and material feeding tube road II also is set on the mixing tank II 5.In the present embodiment, described mixing tank I 3 adopts venturi mixer, and mixing tank II 5 adopts static mixer, and interchanger 4 adopts plate-type heat exchanger.
Utilize said apparatus to be prepared the method for 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution, following two kinds of technical schemes arranged:
The first technical scheme is: in reactor 1, pack in advance account for reactor volume 50% the liquid reacting product that contains the 3-methylthiopropionaldehyde as the circulating reaction medium, start recycle pump 2, drive the circulating reaction medium successively by mixing tank I 3, interchanger 4 and mixing tank II 5 circulate in the Returning reactor 1 again, in working cycle, described circulating reaction medium fully mixes with the thiomethyl alcohol liquid and the catalyzer organic bases that inject by material feeding tube road I in mixing tank I 3, in interchanger 4 through water quench to being lower than reactor 1 interior temperature, in mixing tank II 5, fully mix with the propenal liquid that injects by material feeding tube road II again, enter at last in the reactor 1, reaction generates the 3-methylthiopropionaldehyde under 20～50 ℃ of conditions of temperature, the liquid reacting product that flows out from reactor 1 is shunted after by recycle pump 2, a part enters the subsequent disposal operation as pending crude product by product discharging pipeline, another part continues above-mentioned circulation as the circulating reaction medium and begins simultaneously the next round reaction, and production process is carried out continuously.
The second technical scheme is: in reactor 1, pack in advance account for reactor volume 50% the liquid reacting product that contains the 3-methylthiopropionaldehyde as the circulating reaction medium, start recycle pump 2, drive the circulating reaction medium successively by mixing tank I 3, interchanger 4 and mixing tank II 5 circulate in the Returning reactor 1 again, in working cycle, described circulating reaction medium fully mixes with the propenal liquid that injects by material feeding tube road I in mixing tank I 3, in interchanger 4 through water quench to being lower than reactor 1 interior temperature, in mixing tank II 5, fully mix with the thiomethyl alcohol liquid and the catalyzer organic bases that inject by material feeding tube road II again, enter at last in the reactor 1, reaction generates the 3-methylthiopropionaldehyde under 20～50 ℃ of conditions of temperature, the liquid reacting product that flows out from reactor 1 is shunted after by recycle pump 2, a part enters the subsequent disposal operation as pending crude product by product discharging pipeline, another part continues above-mentioned circulation as the circulating reaction medium and begins simultaneously the next round reaction, and production process is carried out continuously.
The difference of above-mentioned two kinds of technical schemes is the charging sequencing of raw material (thiomethyl alcohol liquid and catalyzer organic bases, propenal liquid).The first technical scheme is that the circulating reaction medium is mixed with thiomethyl alcohol liquid and catalyzer organic bases first, after the cooling again with the propenal liquid mixing; And the second technical scheme is with circulating reaction medium elder generation and propenal liquid mixing, mixes with thiomethyl alcohol liquid and catalyzer organic bases after the cooling again.From purity and the yield of 3-methylthiopropionaldehyde product, more preferably the first technical scheme.
Through the effects, adopt device of the present utility model to prepare the 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution, help to form all reaction systems of relatively stable, equal perseverance of temperature, concentration and a speed of response, can avoid because of thiomethyl alcohol or the propenal partial concn is too high and/or local superheating causes side reaction, reduce by product and generate, improve purity and the yield of 3-methylthiopropionaldehyde product.Concrete experiment condition is: the mol ratio of thiomethyl alcohol liquid and propenal liquid is 1.05, the mol ratio of catalyzer organic bases and thiomethyl alcohol liquid is 800ppm, temperature of reaction is 39 ℃, adopts Shimadzu GC-2014C gas chromatograph that the liquid reacting product that flows out in the reactor discharge port is carried out quantitative and qualitative analysis.Experimental result sees the following form.
Sequence number 1～4 can be found out in the relatively upper table, no matter be to increase separately mixing tank I or mixing tank II, all can improve purity and the yield of 3-methylthiopropionaldehyde product, wherein best with the effect that increases simultaneously mixing tank I and mixing tank II, propenal liquid is more abundant with contacting of thiomethyl alcohol liquid, mix more even, minimizing is because of propenal or the too high side reaction that causes of thiomethyl alcohol partial concn, the content of 3-methylthiopropionaldehyde reaches more than the 95%mol, and yield all reaches more than the 92%mol in thiomethyl alcohol or propenal.Sequence number 4～6 can be found out in the relatively upper table, after in device, further increasing interchanger, can effectively control temperature of charge, reduce the temperature fluctuation in the reactor, be beneficial to all reaction systems of relatively stable, equal perseverance of formation temperature, concentration and speed of response, the side reaction that minimizing causes because of the system local superheating, the content of 3-methylthiopropionaldehyde product can improve approximately 2.5%mol again, and yield can improve approximately 5%mol again in propenal.
Explanation is at last, above preferred embodiment is only unrestricted in order to the technical solution of the utility model to be described, although by the utility model being described with reference to above preferred embodiment, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the spirit and scope of the present utility model that appended claims limits.
Claims (2)
1. prepared the device of 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution, it is characterized in that, comprise reactor, recycle pump, mixing tank I and mixing tank II; The discharge port of described reactor is communicated with the opening for feed of recycle pump, and the discharge port of recycle pump is communicated with the opening for feed of mixing tank I, and the discharge port of mixing tank I is communicated with the opening for feed of mixing tank II, and the discharge port of mixing tank II is communicated with the opening for feed of reactor; Described recycle pump also arranges product discharging pipeline to the path of mixing tank I, material feeding tube road I also is set on the mixing tank I, and material feeding tube road II also is set on the mixing tank II.
2. the device that is prepared the 3-methylthiopropionaldehyde by thiomethyl alcohol and propenal reactive liquid solution according to claim 1, it is characterized in that, described mixing tank I also arranges interchanger to the path of mixing tank II, the opening for feed of interchanger is communicated with the discharge port of mixing tank I, and the discharge port of interchanger is communicated with the opening for feed of mixing tank II.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220440644 CN202766441U (en) | 2012-08-31 | 2012-08-31 | Device for preparing 3-methylthiopropionaldehyde through liquid-liquid reaction of methyl mercaptan and acrolein |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220440644 CN202766441U (en) | 2012-08-31 | 2012-08-31 | Device for preparing 3-methylthiopropionaldehyde through liquid-liquid reaction of methyl mercaptan and acrolein |
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| CN202766441U true CN202766441U (en) | 2013-03-06 |
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| CN 201220440644 Ceased CN202766441U (en) | 2012-08-31 | 2012-08-31 | Device for preparing 3-methylthiopropionaldehyde through liquid-liquid reaction of methyl mercaptan and acrolein |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796030A (en) * | 2012-08-31 | 2012-11-28 | 重庆紫光天化蛋氨酸有限责任公司 | Method and device for preparing 3-methylmercapto-propionaldehyde through liquid-liquid reaction of methyl mercaptan and acraldehyde |
| CN105646302A (en) * | 2016-02-05 | 2016-06-08 | 宁夏紫光天化蛋氨酸有限责任公司 | Production method of methyl mercaptan salt |
-
2012
- 2012-08-31 CN CN 201220440644 patent/CN202766441U/en not_active Ceased
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796030A (en) * | 2012-08-31 | 2012-11-28 | 重庆紫光天化蛋氨酸有限责任公司 | Method and device for preparing 3-methylmercapto-propionaldehyde through liquid-liquid reaction of methyl mercaptan and acraldehyde |
| CN105646302A (en) * | 2016-02-05 | 2016-06-08 | 宁夏紫光天化蛋氨酸有限责任公司 | Production method of methyl mercaptan salt |
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Effective date of registration: 20160526 Address after: 755000 the Ningxia Hui Autonomous Region City Center Industrial Park Patentee after: NINGXIA ZIGUANG TIANHUA METHIONINE CO., LTD. Address before: 408200, Chongqing County, Zhenjiang Town, Fengdu village Xiangjiaba Patentee before: Chongqing Unisplendour Tianhua Methionine Co., Ltd. |
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| IW01 | Full invalidation of patent right |
Decision date of declaring invalidation: 20190531 Decision number of declaring invalidation: 40396 Granted publication date: 20130306 |
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| IW01 | Full invalidation of patent right |