CN205011675U - N - ethyl - N - (3'- sulfonic acid) benzylaniline cleans continuous separation device of production - Google Patents
N - ethyl - N - (3'- sulfonic acid) benzylaniline cleans continuous separation device of production Download PDFInfo
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- CN205011675U CN205011675U CN201520749891.0U CN201520749891U CN205011675U CN 205011675 U CN205011675 U CN 205011675U CN 201520749891 U CN201520749891 U CN 201520749891U CN 205011675 U CN205011675 U CN 205011675U
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Abstract
The utility model relates to a N - ethyl - N - (3'- sulfonic acid) benzylaniline cleans continuous separation device of production, including mixing apparatus, neutralizing device A, splitter A, sedimentation tank, filtration equipment, neutralizing device B, crystallization equipment, splitter B, mother liquor recovery pond that connects gradually and the delivery pump system that links to each other with the pond, retrieve the mother liquor and carry to mixing apparatus through the delivery pump system that links to each other with the pond, neutralizing device A still is provided with parameter detecting device, parameter detecting device be online pH value and temperature measurement control system, neutralizing device B still is provided with parameter and crystal detection device and crystal viewing device, parameter and crystal detection device observe control system on line for online pH value and temperature measurement control system and crystal. The utility model has the advantages of: the utility model discloses an on -line measuring carries out serialization parameter control, makes the continuous crystallization of material, separation to improve the purity and the productivity of product.
Description
Technical field
The device that the material that the utility model relates to a kind of intermediate cleanly production is continuously separated, particularly a kind of N-ethyl-N-(3 ˊ-sulfonic acid) continuous separation device of benzylaniline cleanly production.
Background technology
Matching stain is the dye that in current dye industry, kind is maximum, and the main raw material major part that they use is that market demand is few, kind is many, the intermediate of manufacturing enterprise's small scale, and such feature seriously restricts the technological innovation of most of intermediate; Especially the new millennium is entered, China's dyestuffs industries development is more rapid, output and consumption have become the prostatitis in the world all, and more resource is put to the field of DYE PRODUCTION and deep processing, but still relatively lag behind to the technological innovation in its supporting intermediate field.
Could separate out from solution system when being combined with temperature effective by salting-out effect some material, when the batch reactor analysis of material by routine, the fine particle that early stage generates to be easy to cover by the nascent state material of rear precipitation, be easy to by product to be wrapped in solid like this, have influence on the purity separating out material; If reduce the wrapped problem of by product by changing stirring form, this is also easy to the size having influence on precipitate particle, and this badly influences production capacity and the efficiency of production.
Therefore, research and develop the device that a kind of material that can improve the purity of product and the intermediate cleanly production of production capacity is continuously separated to be necessary.
Utility model content
The technical problems to be solved in the utility model is to provide and a kind ofly can improves the purity of product and the N-ethyl-N-(3 ˊ-sulfonic acid of production capacity) continuous separation device of benzylaniline cleanly production.
For solving the problems of the technologies described above, the technical solution of the utility model is: N-ethyl-N-(3 ˊ-sulfonic acid) continuous separation device of benzylaniline cleanly production, its innovative point is: the drug delivery pump system comprising mixing equipment, neutralizing device, separating device, settling tank, filter plant, crystallizer, disposing mother liquor pond and be connected with pond, described neutralizing device comprises neutralizing device A and B, and separating device comprises separating device A and B; The liquid outlet of described mixing equipment is communicated with the fluid inlet of neutralizing device A, and the liquid outlet of neutralizing device A is communicated with the fluid inlet of separating device A; Described separating device A also comprises discharge port and liquid outlet, the liquid outlet of separating device A is communicated with the fluid inlet of settling tank, the liquid outlet of settling tank is communicated with the fluid inlet of filter plant, the liquid outlet of filter plant is communicated with the fluid inlet of neutralizing device B, the liquid outlet of neutralizing device B is communicated with the fluid inlet of crystallizer, and the liquid outlet of crystallizer is communicated with the fluid inlet of separating device B; Described separating device B also comprises discharge port and liquid outlet, and the liquid outlet of separating device B is communicated with the fluid inlet in disposing mother liquor pond, and Ethylene recov is delivered to mixing equipment by the drug delivery pump system be connected with pond by the liquid outlet in described disposing mother liquor pond.
Further, described neutralizing device A comprises the mixing tank with chuck, and described mixing tank is provided with alkali lye feeding device; Described neutralizing device A is also provided with parameter detection device, and described parameter detection device is on-line pH value and temperature measuring Controlling System.
Further, described neutralizing device B comprises the mixing tank with chuck, and described mixing tank is provided with alkali lye feeding device and crystal seed adding set; Described neutralizing device B is also provided with parameter and crystal proofing unit and Crystal Observation device, and described parameter and crystal proofing unit are that on-line pH value and temperature measuring Controlling System and crystal observe Controlling System online.
The utility model has the advantage of:
(1) sulfonated liquid mixes with the mother liquid coming in mixing equipment according to the amount of regulation, mixed solution carried out adding alkali cooling by the neutralizing device A being fed to parameters proofing unit continuously and continuous discharge to separating device A, isolated liquid carries out flocculation sediment, filtration, the neutralizing device B that clear liquid is continuously fed to parameters detection observing device carries out adding alkali, long crystalline substance, also continuous discharge is to separating device B through crystallizer cooling for brilliant liquid, and the mother liquor of separation returns mixing equipment according to demand; The utility model, by on-line checkingi, carries out serialization state modulator, impels material continuous crystallisation, separation, thus improves purity and the production capacity of product.
(2) in the utility model, neutralizing device A and neutralizing device B is provided with on-line pH value and temperature measuring Controlling System, makes measuring point accurate, and the pH value of detection and temperature are accurately, and safe and reliable, thus make the raising of the purity of product and production capacity more guaranteed; Meanwhile, labour intensity is also made to reduce.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail.
Fig. 1 is the utility model N-ethyl-N-(3 ˊ-sulfonic acid) company of benzylaniline cleanly production
The equipment flowsheet of continuous tripping device.
Embodiment
The following examples can make professional and technical personnel's comprehend the utility model, but are not therefore limited among described scope of embodiments by the utility model.
Embodiment
As shown in Figure 1, in mixing equipment, prepare a collection of mixed solution, stand-by; Open the water coolant of the anterior premix make and break of neutralizing device A, by mixed solution and 40% sodium hydroxide solution respectively measure control carry out Automatic continuous charging at 2153kg/h, 784kg/h, flow into mixing tank simultaneously and carry out the reaction of deacidification degree;
Control through midway on-line detecting system, the flow of fine setting charging and rear disconnected cooling water valve size, adjust pH=1.7, cool to 30 DEG C, mixing suspension enters into separating device A from mixer outlet and carries out feed separation, and parting liquid again sedimentation goes out subparticle;
Parting liquid is by free flow pressure filter, filter out residual material, obtain clarifying containing the metabisulfite solution of a small amount of sulfuric acid, by sodium sulfate liquid and 40% sodium hydroxide solution respectively measure control carry out Automatic continuous charging at 1467kg/h, 85kg/h, flow into neutralizing device B simultaneously and carry out neutralization reaction;
Control through midway on-line detecting system, the flow of fine setting charging and cooling water valve size, adjust pH=7.0, cool to 25 DEG C, be confirmed whether to add oversaturated sodium sulfate (crystal seed) by Crystal Observation device, suspension enters into crystallizer from mixer outlet, cools to 5 DEG C by chilled brine, flow into the separation that separating device B carries out sodium sulfate crystal again, on request the separation mother liquor of 3360kg is returned mixing equipment.
N-ethyl-N-(3 ˊ-the sulfonic acid adopting above-mentioned moving material tripping device to produce) benzylaniline, achieve automatic continuous production, improve the quality of product.
comparative example
In mixing equipment, prepare a collection of mixed solution, be transferred in reactor the sodium hydroxide solution tune pH=1.8 being added dropwise to 40%, cooled to 25 DEG C with 4 hours, enter into separating device A and carry out feed separation, parting liquid again sedimentation goes out subparticle;
Parting liquid, by free flow pressure filter, filters out residual material, flow in reactor the sodium hydroxide solution tune pH=7.0 being added dropwise to 40%, cools to 5 DEG C, then flow into the separation that separating device B carries out sodium sulfate crystal with 4 ~ 6 hours with freezing salt solution.
By the production of this kind of mode, can only produce the material of two batches every day, the purity of intermediate is on average 99%.
Conclusion: the utility model is compared with the intermittent reaction of comparative example, and the purity of intermediate has carried 0.5%, labour intensity reduces by 40%, and production capacity improves 1.5 times.
More than show and describe ultimate principle of the present utility model and principal character and advantage of the present utility model.The technician of the industry should understand; the utility model is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present utility model; under the prerequisite not departing from the utility model spirit and scope; the utility model also has various changes and modifications, and these changes and improvements all fall within the scope of claimed the utility model.The claimed scope of the utility model is defined by appending claims and equivalent thereof.
Claims (3)
1.N-ethyl-N-(3 ˊ-sulfonic acid) continuous separation device of benzylaniline cleanly production, it is characterized in that: the drug delivery pump system comprising mixing equipment, neutralizing device, separating device, settling tank, filter plant, crystallizer, disposing mother liquor pond and be connected with pond, described neutralizing device comprises neutralizing device A and B, and separating device comprises separating device A and B; The liquid outlet of described mixing equipment is communicated with the fluid inlet of neutralizing device A, and the liquid outlet of neutralizing device A is communicated with the fluid inlet of separating device A; Described separating device A also comprises discharge port and liquid outlet, the liquid outlet of separating device A is communicated with the fluid inlet of settling tank, the liquid outlet of settling tank is communicated with the fluid inlet of filter plant, the liquid outlet of filter plant is communicated with the fluid inlet of neutralizing device B, the liquid outlet of neutralizing device B is communicated with the fluid inlet of crystallizer, and the liquid outlet of crystallizer is communicated with the fluid inlet of separating device B; Described separating device B also comprises discharge port and liquid outlet, and the liquid outlet of separating device B is communicated with the fluid inlet in disposing mother liquor pond, and Ethylene recov is delivered to mixing equipment by the drug delivery pump system be connected with pond by the liquid outlet in described disposing mother liquor pond.
2. N-ethyl-N-(3 ˊ-sulfonic acid according to claim 1) continuous separation device of benzylaniline cleanly production, it is characterized in that: described neutralizing device A comprises the mixing tank with chuck, and described mixing tank is provided with alkali lye feeding device; Described neutralizing device A is also provided with parameter detection device, and described parameter detection device is on-line pH value and temperature measuring Controlling System.
3. N-ethyl-N-(3 ˊ-sulfonic acid according to claim 1) continuous separation device of benzylaniline cleanly production, it is characterized in that: described neutralizing device B comprises the mixing tank with chuck, and described mixing tank is provided with alkali lye feeding device and crystal seed adding set; Described neutralizing device B is also provided with parameter and crystal proofing unit and Crystal Observation device, and described parameter and crystal proofing unit are that on-line pH value and temperature measuring Controlling System and crystal observe Controlling System online.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520749891.0U CN205011675U (en) | 2015-09-25 | 2015-09-25 | N - ethyl - N - (3'- sulfonic acid) benzylaniline cleans continuous separation device of production |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520749891.0U CN205011675U (en) | 2015-09-25 | 2015-09-25 | N - ethyl - N - (3'- sulfonic acid) benzylaniline cleans continuous separation device of production |
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| CN205011675U true CN205011675U (en) | 2016-02-03 |
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| CN201520749891.0U Active CN205011675U (en) | 2015-09-25 | 2015-09-25 | N - ethyl - N - (3'- sulfonic acid) benzylaniline cleans continuous separation device of production |
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| TR01 | Transfer of patent right |
Effective date of registration: 20221010 Address after: No. 169, Jingsizhi Road, Baiyang Street, Hangzhou Economic and Technological Development Zone, Hangzhou, Zhejiang 310018 Patentee after: HANGZHOU XIASHA HENGSHENG CHEMICAL CO.,LTD. Address before: No. 258, Shanghai Road, Binjiang Fine Chemical Park, Qidong, Nantong, Jiangsu 226000 Patentee before: HENGSHENG CHEMICAL Co.,Ltd. |
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| TR01 | Transfer of patent right |