CN104086622A - Circulating dephenolizing device and circulating dephenolizing process for producing cottonseed protein by virtue of extraction method - Google Patents

Circulating dephenolizing device and circulating dephenolizing process for producing cottonseed protein by virtue of extraction method Download PDF

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Publication number
CN104086622A
CN104086622A CN201410309183.5A CN201410309183A CN104086622A CN 104086622 A CN104086622 A CN 104086622A CN 201410309183 A CN201410309183 A CN 201410309183A CN 104086622 A CN104086622 A CN 104086622A
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methanol
mother liquor
extraction
dephenolizing
separating box
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CN201410309183.5A
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CN104086622B (en
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卢作文
葛玉梅
于奇
李树平
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XINJIANG TARIM ZHENQI BIOLOGICAL SCIENCE & TECHNOLOGY Co Ltd
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XINJIANG TARIM ZHENQI BIOLOGICAL SCIENCE & TECHNOLOGY Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

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Abstract

The invention relates to a circulating dephenolizing device and a circulating dephenolizing process for producing cottonseed protein by virtue of an extraction method. The device comprises a multistage spray extraction extractor, a precipitation type liquid separating tank, a rectifying tower, a condenser, a methanol mother liquor tank and a mother liquor pipe, wherein an external circulation circuit is arranged between the extractor and the liquid separating tank; an extract liquor recycling pipeline with a regulating valve is arranged between the upper part of a first-stage funnel tank of the extractor and the liquid separating tank; a methanol backflow pipeline is arranged between the lower part of the liquid separating tank and a back spray pipe at the upper part of the first stage of the extractor; a rectifying circuit is arranged between the methanol backflow pipeline and the mother liquor tank. The dephenolizing process comprises the steps of solvent extraction, methanol extraction dephenolization and methanol recycling, wherein the dephenolizing methanol solution coming out of the extractor is subjected to liquid separation via the precipitation type liquid separating tank; the organic solution at the upper part is returned to the extraction work section, a part of the methanol phenol-containing mixed liquor at the lower part returns to the extraction dephenolizing work section to be recycled and the other part of the mixed liquor is rectified, dephenolized and condensed to obtain liquid methanol so as to be recycled. In the dephenoling work section, the energy consumption is saved by 30% and the methanol is saved by above 10%.

Description

Extraction process is produced cottonseed protein circulation dephenolize device and technique thereof
Technical field
The invention belongs to chemical field, relate to a kind of extraction process and produce cottonseed protein device and technique, be specially a kind of extraction process and produce in cottonseed protein, circulate dephenolize device and technique thereof.
Background technology
In cottonseed processing, use organic solvent lixiviate grease, then can obtain feed grade cotton protein with methanol stripper gossypol.Because it is leach at low temperature technique, can guarantee in production process that cotton protein is not because of hyperthermia and superheating sex change.This production method has been substituted traditional hot moulding technique at present becomes conventional production method, can not only obtain Oleum Gossypii semen, and obtain high-quality feed albumen.
In above-mentioned extraction process production technique, for cost-saving, need to organic solvent is separated with grease, methyl alcohol separated with gossypol after, organic solvent and methyl alcohol are carried out to recycle.Separated method is normally utilized the boiling point difference of different phase components that mixed solution is distilled to condensation again and is collected.As the method for the application number disclosed a kind of cottonseed protein extracting process Methanol Recovery of Chinese patent that is 200710014071.7, its step is through strainer by dephenolizing extractor methyl alcohol out, enter skimmer, the oil phase that skimmer separates is delivered to carries oily leacher, the water conveying separating is to temporary tank, aqueous portion pumps into rectifying tower through under meter, through reboiler, reclaims methanol gas.Although this technique can realize the cyclically utilizing of lixiviate medium, methyl alcohol distills, the lifting capacity of boiling is again large, need to consume a large amount of heat energy.
In order further to reduce the heat energy consumption in medium separating and recovering process, lower fractionation by distillation load, need to be optimized design to separating methanol recovery process.
Summary of the invention
The object of the present invention is to provide a kind of methanol loop through optimization to utilize technique, to reduce extraction extraction, produce cotton protein Methanol Recovery energy consumption, improve methyl alcohol utilising efficiency.
Extraction process cottonseed protein circulation dephenolize device of the present invention, comprise multi-stage spray extraction leacher, separating box, rectifying tower, condenser, methanol mother liquor case and mother liquor pipe, every grade of spraying and extracting leaches unit and includes shower, end sieve tray dish, funnel case, Sprayer Circulation pump and Sprayer Circulation pipe, funnel cases at different levels top is communicated with, and according to material direct of travel edge, raise step by step, mother liquor pipe is connected respectively with Sprayer Circulation pipes at different levels.Described separating box is precipitation, establishes overflow port, the recovery mouth with gate valve is established in bottom on the top of separating box end.Between described leacher and separating box, form external circulation, this external circulation structure is: between the first step funnel case top of leacher and separating box, establish the extraction liquid recycling pipeline with variable valve, returning between jet pipe of separating box bottom and leacher first step top arranges methanol eddy pipeline, and is equipped with recycle pump on recycling pipeline and return line.Between methanol eddy pipeline and mother liquor case, rectifying loop is set, this rectifying loop is comprised of rectifying variable valve, rectifying tower, condenser.Condenser is connected with mother liquor case.Between mother liquor pipe and Sprayer Circulation pipe at different levels, mother liquor variable valve is set.
Described separating box inside is established the unconnected vertical baffle of two-stage and top casing is divided into three parts, and extraction liquid recycling pipeline end is in first part, and the initiating terminal of methanol eddy pipeline is at second section, and overflow port, recovery mouth are in third part.First step dividing plate is higher than second stage dividing plate, and establishes separating tube on first step dividing plate.In separating box, the end of recycling pipeline arranges buffer cap.
Apply the circulation dephenolizing process of circulation dephenolize device as above, comprise extraction, methyl alcohol dephenolize, Methanol Recovery utilization.Described Methanol Recovery utilization is through precipitation separating box separatory from leacher dephenolize methanol solution out, the top organic solution of getting is returned to lixiviate workshop section, and the methyl alcohol of bottom returns to the first step recycle of extracting and dephenolizing workshop section containing a phenol mixed solution part, another part obtains liquid methanol after condensation again through rectifying dephenolize, returns to the recycle of methanol mother liquor case.
Adopt after device and technique as above, methyl alcohol dephenolize solution is not only in lixiviate section at different levels recycle, and its mixed solution is because thereby concentration of component gradient disparities forms the anti-stream contrary with material direct of travel between funnel cases at different levels, to the top of first step funnel case, be exported.Mixed solution is separated at settler, and the top organic solution obtaining is returned to lixiviate workshop section, and the phenol solution part that contains of bottom is directly returned to supply dephenolizing extractor, and another part returns to methanol mother liquor case after gossypol is removed in rectifying.
The loop between precipitation separating box and dephenolizing extractor has been constructed in this invention, and what make to remove after precipitate and separate organic solvent directly returns to lixiviate dephenolize containing phenol methanol solution, obtains recycle.Simplify the process procedure that Methanol Recovery is purified and recycled, shortened operational path.Make processing unit compacter, save Methanol Recovery energy consumption, reduce the loss in Methanol Recovery stage, reduce costs.
Accompanying drawing explanation
Fig. 1 is that extraction process of the present invention is produced cottonseed protein circulation dephenolize apparatus structure schematic diagram.
Fig. 2 is that extraction process of the present invention is produced cottonseed protein circulation dephenolizing process schema.
Embodiment
As Fig. 1 and Fig. 2, extraction process cottonseed protein circulation dephenolize device, comprises multi-stage spray extraction leacher 1, separating box 2, rectifying tower 9, condenser 19, methanol mother liquor case 3 and mother liquor pipe 13.Every grade of spraying and extracting leaches unit and comprises shower 12, end sieve tray dish 21, funnel case 5, Sprayer Circulation pump 16 and Sprayer Circulation pipe 15.Funnel cases at different levels 5 tops are communicated with, and raise step by step according to material direct of travel edge., mother liquor pipe 13 is connected respectively with Sprayer Circulation pipes 15 at different levels.
Between described leacher 1 and separating box 2, form external circulation, this external circulation structure is: between first step funnel case 5 tops of leacher 1 and separating box 2, establish the extraction liquid recycling pipeline 6 with variable valve 8, returning between jet pipe 11 of separating box 2 bottoms and leacher 1 first step top arranges methanol eddy pipeline 22, and is equipped with recycle pump 26 on recycling pipeline 6 and return line 22.
Between methanol eddy pipeline 22 and mother liquor case 3, rectifying loop is set, this rectifying loop is comprised of rectifying variable valve 7, rectifying tower 9, condenser 19, and condenser 19 is connected with mother liquor case 3.Between mother liquor pipe 13 and Sprayer Circulation pipe 15 at different levels, mother liquor variable valve 14 is set.
Described separating box 2 is precipitation, and separating box 2 inside establish two-stage and the unconnected vertical baffle 4a in top, 4b are divided into three parts by casing.Extraction liquid recycling pipeline 6 ends are in first part, and the initiating terminal of methanol eddy pipeline 22 is in the bottom of second section, and overflow port 17, recovery mouth 1 lay respectively at the upper and lower of third part.First step dividing plate 4a is higher than second stage dividing plate 4b, and establishes separating tube 10 on first step dividing plate 4a.The mixed solution that enters casing obtains stable and preliminary sedimentation layering in first part, and the organic solution on top climbs over dividing plate 4a and enters casing second section, and separating tube 10 imports the methanol solution of bottom at the middle part of second section.Mixed solution is in the further precipitate and separate of second section, and the organic solution on top climbs over dividing plate 4b and enters third part, and the phenol solution that contains of bottom enters return line 22.In third part, further the organic solution after precipitate and separate is collected from overflow port 17 the lixiviate workshop section directly returning in dephenolize, the methanol solution of bottom deposition temporary and after reaching finite concentration from reclaiming mouthful 1 pump to rectifying loop.The end of the recovery tube 6 in separating box 2 first parts arranges buffer cap 20, can make liquid phase stable as early as possible.
Material right-to-left on end sieve tray dish 21 is advanced in way step by step, in sprays at different levels unit, is sprayed step by step.Gossypol in material reduces step by step, thereby the methyl alcohol mixed liquor that contains organic solvent, gossypol is because concentration of component gradient disparities forms the anti-stream contrary with material direct of travel between funnel cases 5 at different levels, to the top of first step funnel case 5, is exported.Mixed solution is in settler 2 separation afterwards, and the top organic solution obtaining is returned to lixiviate workshop section, and the phenol solution part that contains of bottom is directly returned to supply dephenolizing extractor 1, and another part returns to methanol mother liquor case 3 after gossypol is removed in rectifying loop.
Utilize the variable valve 8 in extraction liquid recycling pipeline 6 can control the ratio that reclaims flow and circulation dephenolize flows at different levels.In like manner, utilize rectifying variable valve 7 to control to enter rectifying loop and directly enter the flow proportional containing phenol solution of extraction unit 1, in the present embodiment, both ratios are about 1:3.Again in like manner, utilize mother liquor variable valve 14 can control methanol mother liquor in the circulation tube 15 of lixiviate dephenolizes at different levels unit and the supply ratio of circulate soln, and alternation step by step, the ratio of specifically supplying with mother liquor declines step by step.
By increasing extract mixed solution recycling pipeline 6 flow, strengthen in rectifying loop containing the flow proportional of phenol solution, can make the content of gossypol in cottonseed protein constantly reduce.And due to the design in methanol loop loop, the supply consumption of fresh methanol is reduced.Reaching under cottonseed protein free phenol≤400ppm prerequisite, dephenolize workshop section energy efficient 30%, saves methyl alcohol more than 10%.Protein content >=50% in the cotton protein of producing, organic solvent≤500ppm, methyl alcohol≤800ppm.

Claims (3)

1. an extraction process cottonseed protein circulation dephenolize device, comprise multi-stage spray extraction leacher (1), separating box (2), rectifying tower (9), condenser (19), methanol mother liquor case (3) and mother liquor pipe (13), every grade of spraying and extracting leaches unit and comprises shower (12), end sieve tray dish (21), funnel case (5), Sprayer Circulation pump (16) and Sprayer Circulation pipe (15); Funnel cases at different levels (5) top is communicated with, and raises step by step according to material direct of travel edge, and mother liquor pipe (13) is connected respectively with Sprayer Circulation pipes at different levels (15); Described separating box (2) is precipitation, establishes overflow port (17), the recovery mouth (18) with gate valve is established in bottom on the top of separating box (2) end; This dephenolize device is characterised in that:
A. between described leacher (1) and separating box (2), form external circulation, this external circulation structure is: between first step funnel case (5) top of leacher (1) and separating box (2), establish the extraction mixed solution recycling pipeline (6) with variable valve (8), returning between jet pipe (11) of separating box (2) bottom and leacher (1) first step top arranges containing phenol methanol eddy pipeline (22), and is equipped with recycle pump (26) on recycling pipeline (6) and return line (22);
B. between methanol eddy pipeline (22) and mother liquor case (3), rectifying loop is set, this rectifying loop is comprised of rectifying variable valve (7), rectifying tower (9), condenser (19), and condenser (19) is connected with mother liquor case (3);
C. between mother liquor pipe (13) and Sprayer Circulation pipe at different levels (15), mother liquor variable valve (14) is set.
2. circulation dephenolize device as claimed in claim 1, separating box (2) inside described in it is characterized in that is established the unconnected vertical baffle of two-stage and top (4a, 4b) casing is divided into three parts, above-mentioned extraction mixed solution recycling pipeline (6) end is in first part, contain the initiating terminal of phenol methanol eddy pipeline (22) at second section, overflow port (17), recovery mouthful (18) are in third part; First step dividing plate (4a) is higher than second stage dividing plate (4b), and on first step dividing plate (4a), establishes separating tube (10); In separating box (2), the end of recycling pipeline (6) arranges buffer cap (20).
One kind application circulation dephenolize device as claimed in claim 1 or 2 technique, comprise extraction, methyl alcohol dephenolize, Methanol Recovery utilization, it is characterized in that described Methanol Recovery utilization is through precipitation separating box separatory from leacher methanol mixed solution out, the top organic solution of getting is returned to the organic lixiviate workshop section before dephenolize, and bottom containing a phenol methyl alcohol mixed liquor part, return to the first step recycle of extracting and dephenolizing workshop section, another part obtains liquid methanol after condensation again through rectifying dephenolize, returns to the recycle of methanol mother liquor case.
CN201410309183.5A 2014-07-01 2014-07-01 Extraction production cottonseed protein circulation dephenolize device and its technique Expired - Fee Related CN104086622B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107410664A (en) * 2016-07-18 2017-12-01 湖南欣瑞生物科技有限公司 A kind of extraction equipment of cottonseed protein

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050147722A1 (en) * 2003-03-12 2005-07-07 Gao Wen Fan Integrated process for separation of oil, protein, carbohydrates, shell and minor toxic components from seeds
CN201433185Y (en) * 2009-07-03 2010-03-31 北京华康希望生物科技有限公司 Complete sets of equipment for cottonseed pretreatment and extraction production of dephenolization cottonseed protein
CN102851113A (en) * 2011-12-09 2013-01-02 湖南省丰康生物科技股份有限公司 Treatment method and device for oil extraction and dephenolization of cottonseed
CN203999457U (en) * 2014-07-01 2014-12-10 新疆塔里木震企生物科技有限公司 Extraction process is produced cottonseed protein circulation dephenolize device

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050147722A1 (en) * 2003-03-12 2005-07-07 Gao Wen Fan Integrated process for separation of oil, protein, carbohydrates, shell and minor toxic components from seeds
CN201433185Y (en) * 2009-07-03 2010-03-31 北京华康希望生物科技有限公司 Complete sets of equipment for cottonseed pretreatment and extraction production of dephenolization cottonseed protein
CN102851113A (en) * 2011-12-09 2013-01-02 湖南省丰康生物科技股份有限公司 Treatment method and device for oil extraction and dephenolization of cottonseed
CN203999457U (en) * 2014-07-01 2014-12-10 新疆塔里木震企生物科技有限公司 Extraction process is produced cottonseed protein circulation dephenolize device

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107410664A (en) * 2016-07-18 2017-12-01 湖南欣瑞生物科技有限公司 A kind of extraction equipment of cottonseed protein

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