CN102335573A - Caprolactam causticization device - Google Patents

Caprolactam causticization device Download PDF

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Publication number
CN102335573A
CN102335573A CN201010234635XA CN201010234635A CN102335573A CN 102335573 A CN102335573 A CN 102335573A CN 201010234635X A CN201010234635X A CN 201010234635XA CN 201010234635 A CN201010234635 A CN 201010234635A CN 102335573 A CN102335573 A CN 102335573A
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China
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ammonia
venturi tube
caprolactam
diameter
causticization
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CN201010234635XA
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CN102335573B (en
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雍玉梅
杨超
王志侃
毛在砂
仇振华
李向阳
姜惠文
张广积
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Sinopec Shijiazhuang Refining & Chemical Co ltd
China Petroleum and Chemical Corp
Institute of Process Engineering of CAS
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Sinopec Shijiazhuang Refining & Chemical Co ltd
China Petroleum and Chemical Corp
Institute of Process Engineering of CAS
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Abstract

The invention provides a caprolactam causticization device, which is mainly composed of a causticization reactor, a circulating pump, a venture type gas mixer and a mother liquor circulation pipeline. The venture type gas mixer contains a Venturi tube, 2-16 ammonia nozzles and an annular ammonia distributor pipe, wherein the annular ammonia distributor pipe is connected with the throat of the Venturi tube through the ammonia nozzles. Ammonia is uniformly added into the Venturi tube through an annular ammonia distributor and the ammonia nozzles. By the venture principle, ammonia is rapidly mixed with a mother liquor in the Venturi tube and is absorbed. The direct absorption and mixing effect by the venture type gas mixer is better than the mixing effect by an ammonia-water absorption tower and a static mixer, thus simplifying technological process, minimizing water consumption, reducing investment cost and saving work space.

Description

A kind of caprolactam causticization device
Technical field
The invention belongs to the refining separation technology field of chemical products, be specifically related to a kind of device that the caprolactam product causticization is handled that is used for.
Background technology
Produce in the caprolactam process in the SNIA method; Must carry out causticization to acid amides oil with ammoniacal liquor and handle, make the acidic by-products salinization in the acid amides oil, improve its affinity water; So that in extraction process, separate, obtain qualified caprolactam finished product through further subtractive process again.Existing causticization technology mainly contains five steps shown in Figure of description 2: 1. on the ammoniacal liquor absorption tower ammonia is dissolved in the water, forms ammonia spirit, through the effusion ammonia of balance pipe ejecting/collecting.2. ammonia spirit carries out liquid liquid with mother liquor at static mixer and mixes.3. take ammonia away at heat exchanger and absorb heat.4. acid amides oil and ammoniacal liquor carry out causticizing reaction in causticization reactor.5. provide power to form the mother liquor forced circulation by circulating pump.The used ammoniacal liquor of causticizing reaction need use the ammonia G&W in the ammoniacal liquor absorption tower, to form ammonia spirit, and equipment needed thereby has absorption tower, ammonia skirt, water skirt and four parts of gas equalizing line, and technological process is tediously long, complicated.The certain water yield of causticization process process need is dissolved ammonia, and water consumption is big; The ammoniacal liquor absorption tower is taken up an area of big, needs certain working space; Static mixer causes pipe resistance big, and power consumption is high.
Application number is that 200910076604 application for a patent for invention discloses a kind of causticization method for acidamide oil,, as caustic caustic and acid amides oil is added in the causticization reactor with the slurry of calcium hydroxide and water preparation, mixes stirring, the product slurry that obtains; The product slurry is directly carried out the extract and separate operation, and perhaps the oil of the acid amides after Separation of Solid and Liquid obtains causticization carries out the extract and separate operation again.This patent is a caustic with calcium hydroxide, has reduced the cost of caustic, but unresolved ammonia absorbs problem.The Venturi tube that Chinese patent CN201001378Y discloses a kind of beverage mixer sucks CO 2System, the technical problem of solution dope CO in the liquid 2Do not find at present to use in the caprolactam production Venturi tube to carry out the patent and the scientific and technical literature report of the mixing and the absorption of ammonia and liquid as yet.
Summary of the invention
The present invention is intended to solve the deficiency of existing caprolactam ammonia causticization technology, and a kind of caprolactam causticization device is provided, and ammonia is directly added closed circuit; Absorb ammonia with the water in the pipeline solution; Simplify ammonia and absorb flow process, reduce equipment investment and power consumption, improve the causticizing reaction effect.
Caprolactam causticization device provided by the invention mainly is made up of causticization reactor, circulating pump, ammonia blended absorbent device and Recycling Mother Solution pipeline.Ammonia blended absorbent device is a Venturi tube mixer, and Venturi tube mixer comprises Venturi tube, 2~16 ammonia nozzles, annular ammonia distributor pipe, and said annular ammonia distributor pipe is connected to Venturi tube throat through the ammonia nozzle.
The diameter of Venturi tube entrance is identical with the Recycling Mother Solution pipeline diameter, and the Recycling Mother Solution pipeline diameter is D, the length h5=0.5 of Venturi tube entrance~2.0D.Venturi tube throat diameter d=0.2~0.8D, the length h3=0.8 of Venturi tube throat~1.5d.The length h4=2.0 of Venturi tube contraction section~4.0 (D-d), venturi contraction section angle β=10 °~30 °.Angle=5 of Venturi tube expansion segment (8) °~20 °, the length of Venturi tube expansion segment confirm according to the expansion segment angle, for: h2=(D/d-1.0) * d/2 * ctg (α/2).The diameter of Venturi tube outlet section is 1.0~2.0 times of diameter of Recycling Mother Solution pipeline, venturi exit length h1=0.8~3.0D.The diameter of annular ammonia distributor pipe confirms that according to the flow velocity of ammonia in annular ammonia distributor pipe the control flow velocity is 10~30m/s.The length of ammonia nozzle is 0.3~0.5d, and the diameter of ammonia nozzle confirms that according to the flow velocity in the ammonia nozzle control flow velocity is 20~60m/s.Diameter d 4=0.05~the 1.0D of the floss hole that the annular ammonia distributes; The diameter of ammonia inlet tube confirms that according to the flow velocity of ammonia in the inlet duct control flow velocity is 10~30m/s.For guaranteeing that ammonia adds in the circulation line smoothly, the ammonia discharge pressure is than the high 10~70kPa of closed circuit pressure.
Ammonia blended absorbent device of the present invention adopts Venturi tube, and is furnished with annular ammonia distributor and ammonia nozzle.Ammonia evenly joins in the Venturi tube through annular ammonia distributor and ammonia nozzle; Utilize the principle of venturi; Ammonia mixes with mother liquor fast in Venturi tube and is absorbed, and has saved ammonia absorption tower and static mixer, has simplified technological process; Reduce cost of investment, reduce floor space.Mensuration result shows; Ammonia is superior to ammoniacal liquor absorption tower device and static mixer through the effect that Venturi tube mixer directly absorbs mixing; Venturi tube mixer directly is connected the Recycling Mother Solution pipeline; Utilize that the water in the solution absorbs ammonia in the pipeline, need not to add in addition entry and absorb ammonia, reduced the consumption of water.Ammonia blended absorbent device utilizes the Venturi tube characteristic, and resistance loss of pipeline is little, and energy consumption is low.
Description of drawings
Fig. 1 is a caprolactam causticization device schematic flow sheet of the present invention;
Fig. 2 is a prior art caprolactam causticization device schematic flow sheet;
Fig. 3 is a Venturi tube mixer structure chart of the present invention;
Fig. 4 is the A-A figure of Fig. 3.
Wherein:
1-heat exchanger, 2-Venturi tube mixer, 3-circulating pump, 4-causticization reactor, 5-static mixer, 6-ammoniacal liquor absorption tower, 7-Venturi tube outlet section, 8-Venturi tube expansion segment, 9-Venturi tube throat, 10-annular ammonia distributor pipe, 11-. ammonia nozzle, 12-Venturi tube contraction section, 13-Venturi tube entrance, 14-ammonia inlet tube, 15-distributor pipe floss hole, 16-Recycling Mother Solution pipeline, D-Recycling Mother Solution pipeline diameter, d-Venturi tube throat diameter, d1-ammonia inlet tube diameter, d2-ammonia nozzle diameter, d3-annular ammonia distributor pipe diameter, d4-distributor pipe floss hole diameter, h1-Venturi tube outlet section height, h2-Venturi tube expansion segment height, h3-Venturi tube throat height, h4-Venturi tube contraction section height, h5-Venturi tube entrance height.
The specific embodiment
Below in conjunction with accompanying drawing the present invention is further described.
Embodiment 1
Caprolactam causticization device of the present invention is as shown in Figure 1, mainly is made up of causticization reactor 4, circulating pump 3, Venturi tube mixer 2 and Recycling Mother Solution pipeline 16.Like Fig. 3, shown in Figure 4, Venturi tube mixer comprises Venturi tube, 8 ammonia nozzles 11, annular ammonia distributor pipe 10, and annular ammonia distributor pipe is connected to the pipe throat 9 of Venturi tube through the ammonia nozzle.The diameter D of Recycling Mother Solution pipeline is 20cm, and Venturi tube entrance diameter is got 20cm, and entrance length is got 30cm (1.5D).The Venturi tube throat diameter is got 10cm (d=0.5D), and throat length is got 10cm; Contraction section length is got 27cm, and the contraction section angle is 21 °.The angle of Venturi tube expansion segment is got 8 °, and expansion segment length is got 72cm.Venturi tube outlet section diameter is got 20cm, and exit length is got 30cm.The diameter of annular ammonia distributor pipe is 20cm; Ammonia inlet tube diameter is got 5cm, guarantees about the speed 20m/s of ammonia in pipeline.The ammonia nozzle that 8 diameters are 1cm is evenly distributed on circumference, and annular ammonia distributor is connected to Venturi tube throat through the ammonia nozzle.The ammonia intake line is equipped with check (non-return) valve, in case ammonia flows backwards.
The operating process of caprolactam causticization device of the present invention does; Directly introduce Venturi tube mixer 2 by the ammonia pipeline and carry out the ammonia blended absorbent; The power in forced circulation loop is provided by circulating pump 3; Ammonia and mother liquor continue blended absorbent in Recycling Mother Solution pipeline 16, get into then to carry out causticizing reaction in the causticization reactor 4, and heat exchanger 1 is taken ammonia away and absorbed heat and causticizing reaction heat.Being operating as of Venturi tube mixer: ammonia enters into annular ammonia distributor pipe 10 by ammonia inlet tube 14; Get into Venturi tube throat 9 through ammonia nozzle 11; Ammonia in Venturi tube throat is recycled the mother liquor absorption; Circulating mother liquor continuously flows into Venturi tube entrance 13 by the powered mother liquor that circulating pump 3 produces, and the Venturi tube of flowing through successively contraction section 12, Venturi tube throat 9, Venturi tube expansion segment flow out through Venturi tube outlet section 7 then.After leaving Venturi tube mixer, circulating mother liquor continues the ammonia in the absorption mother liquor.The present embodiment ammonia flow is 182kg/h, flows backwards for avoiding ammonia, and the ammonia input pressure must be higher than closed circuit Venturi tube inlet pressure 23kPa.Through measuring, the ammonia absorptivity reaches 97%, and the causticization reactor top is measured the effusion ammonia concentration and is lower than 3%, saves to absorb 1 ton/hour of ammonia water, the also corresponding reduction of the pressure loss of closed circuit.
Embodiment 2
Other type of the present invention, annular ammonia distributor pipe diameter is 1cm; Ammonia inlet tube diameter is got 0.25cm, and ammonia gets into the speed of mixing apparatus in 1~5m/s range regulation; The nozzle that 4 diameters are 1cm is evenly distributed on circumference, connects Venturi tube throat and annular ammonia distributor, and the resistance of blast tube is that circulating pipe distributes 10 times of resistances, can ammonia be evenly distributed to 4 nozzles.Acid amides oil is taken from Shijiazhuang refinery Petrochemical Company worker division department of China Petrochemical Industry caprolactam device.It is 0.5~1kg/h that ammonia adds inbound traffics.
For the mixed effect of check Venturi tube mixer, causticization reactor 4 top free ammonia concentration are measured.Through measuring.When the ammonia flow that feeds was 1.0kg/h, its absorptivity can reach 98%; Along with the minimizing of ammonia flow, the ammonia absorptivity constantly increases; When ammonia flow was 0.5kg/h, the ammonia absorptivity can reach 99.5%, and ammonia approaches to absorb fully in reactor, and it is good to explain that ammonia of the present invention absorbs mixed effect.
As relatively, the causticization reactor 4 top free ammonia concentration of prior art also to be measured, the flow process of caprolactam causticization device is as shown in Figure 2.The concentration that ammoniacal liquor absorption tower 6 generates ammoniacal liquor is 20%, and ammoniacal liquor mixes with acid amides oil through static mixer 5, gets into causticization reactor then and carries out causticizing reaction, and the ammoniacal liquor range of flow is about 2.5~5L/h.Through measuring; The concentration of the free ammonia at causticization reactor 4 tops is 2%, should technology ammonia absorptivity be 98% promptly, and the result who directly adds Venturi tube with ammonia of the present invention is suitable; But the method that adopts Venturi tube directly to add ammonia can be saved and absorbed ammonia water 2.5~5kg/h; And the pressure loss of closed circuit reduces 3%, has practiced thrift power consumption, helps environmental protection.

Claims (9)

1. caprolactam causticization device; Mainly form by causticization reactor (4), circulating pump (3), ammonia blended absorbent device and Recycling Mother Solution pipeline (16); It is characterized in that: said ammonia blended absorbent device is Venturi tube mixer (2); Said Venturi tube mixer comprises Venturi tube, 2~16 ammonia nozzles (11), annular ammonia distributor pipe (10), and said annular ammonia distributor pipe is connected to Venturi tube pipe throat (9) through the ammonia nozzle.
2. caprolactam causticization device according to claim 1 is characterized in that: the diameter of Venturi tube entrance (13) is identical with Recycling Mother Solution pipeline (16) diameter, and the Recycling Mother Solution pipeline diameter is D, the length h5=0.5 of Venturi tube entrance~2.0D.
3. caprolactam causticization device according to claim 1 is characterized in that: the Venturi tube throat diameter is d, d=0.2~0.8D, the length h3=0.8~1.5d of Venturi tube throat (9).
4. caprolactam causticization device according to claim 1 is characterized in that: the length of Venturi tube contraction section (12): h4=2.0~4.0 (D-d), venturi contraction section angle (β) are 10 °~30 °.
5. caprolactam causticization device according to claim 1 is characterized in that: angle=5 of Venturi tube expansion segment (8) °~20 °, the length of Venturi tube expansion segment (h2) is h2=(D/d-1.0) * d/2 * ctg (α/2).
6. caprolactam causticization device according to claim 1 is characterized in that: the diameter of Venturi tube outlet section (7) is 1.0~2.0 times of diameter of Recycling Mother Solution pipeline 16, venturi exit length: h1=0.8~3.0D.
7. caprolactam causticization device according to claim 1 is characterized in that: the diameter of ammonia distribution ring pipe 10 confirms that according to the flow velocity of ammonia in ammonia distribution ring pipe the control flow velocity is 10~30m/s.
8. caprolactam causticization device according to claim 1 is characterized in that: the ammonia nozzle length is 0.3~0.5d, and the diameter of ammonia nozzle (11) confirms that according to the flow velocity in the ammonia nozzle control flow velocity is 20~60m/s.
9. caprolactam causticization device according to claim 1 is characterized in that: the diameter d 4=0.05~1.0D of the floss hole of annular ammonia distributor pipe (15); The diameter (d1) of ammonia inlet tube (14) confirms that according to the flow velocity of ammonia in the inlet duct control flow velocity is 10~30m/s.
CN 201010234635 2010-07-23 2010-07-23 Caprolactam causticization device Active CN102335573B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102631850A (en) * 2012-05-07 2012-08-15 三明中环科经贸有限公司 Gas mixer
CN102921370A (en) * 2012-11-08 2013-02-13 广西华纳新材料科技有限公司 Venturi tube reactor
CN103316621A (en) * 2013-07-22 2013-09-25 河北冀衡化学股份有限公司 Method for preparing trichloroisocyanuric acid by using pipeline reactor
CN106422994A (en) * 2016-10-21 2017-02-22 北京沃特尔水技术股份有限公司 Method and device for preparing ammonium carbonate extraction solution
CN107763626A (en) * 2017-11-17 2018-03-06 厦门大学 Ammonia fuel mixer
CN108714376A (en) * 2018-05-21 2018-10-30 山东新和成氨基酸有限公司 A kind of venturi mixer of the cavity containing porous annular and its application in synthesizing cyanalcohol

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50115949U (en) * 1974-03-07 1975-09-22
GB1411061A (en) * 1972-01-27 1975-10-22 Snia Viscosa Method for the production of omega lactams and their precursors by formation and nitrosation of a cyclomethylene ketene-so2 adduct
GB1430006A (en) * 1972-06-28 1976-03-31 Snia Viscosa Method of extracting lactams from acidic reaction mixtures
CN1629143A (en) * 2004-09-24 2005-06-22 中国石油化工股份有限公司 Process for extracting and separating caprolactam from amide oil
CN101481351A (en) * 2009-01-09 2009-07-15 清华大学 Causticization method for acidamide oil
CN101596437A (en) * 2008-06-03 2009-12-09 中国科学院过程工程研究所 A kind of fluid distributor that is applicable to the heterophase reactor of toluene method caprolactam technology

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1411061A (en) * 1972-01-27 1975-10-22 Snia Viscosa Method for the production of omega lactams and their precursors by formation and nitrosation of a cyclomethylene ketene-so2 adduct
GB1430006A (en) * 1972-06-28 1976-03-31 Snia Viscosa Method of extracting lactams from acidic reaction mixtures
JPS50115949U (en) * 1974-03-07 1975-09-22
CN1629143A (en) * 2004-09-24 2005-06-22 中国石油化工股份有限公司 Process for extracting and separating caprolactam from amide oil
CN101596437A (en) * 2008-06-03 2009-12-09 中国科学院过程工程研究所 A kind of fluid distributor that is applicable to the heterophase reactor of toluene method caprolactam technology
CN101481351A (en) * 2009-01-09 2009-07-15 清华大学 Causticization method for acidamide oil

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102631850A (en) * 2012-05-07 2012-08-15 三明中环科经贸有限公司 Gas mixer
CN102631850B (en) * 2012-05-07 2014-03-26 三明中环科经贸有限公司 Gas mixer
CN102921370A (en) * 2012-11-08 2013-02-13 广西华纳新材料科技有限公司 Venturi tube reactor
CN102921370B (en) * 2012-11-08 2014-09-10 广西华纳新材料科技有限公司 Venturi tube reactor
CN103316621A (en) * 2013-07-22 2013-09-25 河北冀衡化学股份有限公司 Method for preparing trichloroisocyanuric acid by using pipeline reactor
CN106422994A (en) * 2016-10-21 2017-02-22 北京沃特尔水技术股份有限公司 Method and device for preparing ammonium carbonate extraction solution
CN107763626A (en) * 2017-11-17 2018-03-06 厦门大学 Ammonia fuel mixer
CN107763626B (en) * 2017-11-17 2023-12-01 厦门大学 Ammonia fuel mixing device
CN108714376A (en) * 2018-05-21 2018-10-30 山东新和成氨基酸有限公司 A kind of venturi mixer of the cavity containing porous annular and its application in synthesizing cyanalcohol
CN108714376B (en) * 2018-05-21 2020-08-18 山东新和成氨基酸有限公司 Venturi mixer containing porous annular cavity and application of venturi mixer in synthesizing cyanohydrin

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