CN104086622B - Extraction production cottonseed protein circulation dephenolize device and its technique - Google Patents

Extraction production cottonseed protein circulation dephenolize device and its technique Download PDF

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Publication number
CN104086622B
CN104086622B CN201410309183.5A CN201410309183A CN104086622B CN 104086622 B CN104086622 B CN 104086622B CN 201410309183 A CN201410309183 A CN 201410309183A CN 104086622 B CN104086622 B CN 104086622B
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methanol
dephenolize
extraction
separating box
mother liquor
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CN104086622A (en
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卢作文
王明亮
葛玉梅
于奇
李树平
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Xinjiang Jinguyuan Biological Technology Co Ltd
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Xinjiang Jinguyuan Biological 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

Extraction production cottonseed protein circulation dephenolize device and technique, including multi-stage spray extraction infuser, precipitating type separating box, rectifying column, condenser, methanol mother liquor case and mother liquor pipe, external circulation is set between described infuser and separating box, the extract recovery pipe with regulating valve is set between the first order funnel upper box part and separating box of infuser, methanol eddy pipeline is set between separating box bottom and time jet pipe on infuser first order top.Rectifying loop is set between methanol eddy pipeline and mother liquor case.The dephenolizing process includes extraction, methanol extraction dephenolize, Methanol Recovery utilization.The dephenolize methanol solution come out from infuser passes through precipitation separating box point liquid, top organic solution returns to extraction workshop section, and methanol mixed liquor containing a phenol part for bottom returns to recycling for extracting and dephenolizing workshop section, another part obtains liquid methanol recycling after rectifying dephenolize is condensed again.Dephenolize workshop section saves energy consumption 30%, saves methanol more than 10%.

Description

Extraction production cottonseed protein circulation dephenolize device and its technique
Technical field
The invention belongs to chemical field, it is related to a kind of extraction production cottonseed protein device and technique, is specially a kind of extraction Follow the example of circulation dephenolize device and its technique in production cottonseed protein.
Background technology
Grease is extracted with organic solvent in cottonseed processing, again with methanol removing techniques can obtain feed grade cotton protein.By In its be low temperature extracting technology, it is ensured that cotton protein is not denatured because of hyperthermia and superheating in production process.The current production method Traditional hot moulding technique instead of as conventional production process, cottonseed oil can not only have been obtained, and obtain high-quality feed egg In vain.
In above-mentioned extraction production technology, be it is cost-effective, it is necessary to organic solvent is separated with grease, methanol and cotton After phenol separation, organic solvent and methanol are recycled.The method of separation typically utilizes the boiling point of different phase components not Collection is condensed again with mixed liquor is distilled.A kind of cottonseed as disclosed in the Chinese patent of Application No. 200710014071.7 The method of protein extracting process Methanol Recovery, its step is that the methanol for coming out dephenolizing extractor passes through filter, into a point liquid Device, the oil phase that knockout is separated, which is delivered to, carries oily infuser, the water conveying separated to temporary storage tank, and aqueous portion is through flowmeter Rectifying column is pumped into, methanol gas is reclaimed through reboiler.Although the technique can realize the circulating and recovering of extraction medium, methanol steams Evaporate, boil load again greatly, it is necessary to consume a large amount of heat energy.
In order to be able to further reduce the thermal energy consumption during medium separating and recovering, lower separated load, it is necessary to right Separating methanol recovery process optimizes design.
The content of the invention
Technique is utilized it is an object of the invention to provide a kind of optimized methanol loop, to reduce extraction extraction production Cotton protein Methanol Recovery energy consumption, improves methanol utilization ratio.
The extraction cottonseed protein circulation dephenolize device of the present invention, including multi-stage spray extraction infuser, separating box, rectifying Tower, condenser, methanol mother liquor case and mother liquor pipe, every grade of spraying and extracting, which leaches unit, includes shower, bottom sieve pallet, funnel Case, Sprayer Circulation pump and Sprayer Circulation pipe, funnel upper box part connections at different levels, and raised step by step according to material direct of travel edge, Mother liquor pipe is respectively connected with leading to Sprayer Circulation pipes at different levels.The separating box is precipitating type, and overflow is set on the top of separating box end Mouth, bottom set the recovery port with gate valve.External circulation is constituted between described infuser and separating box, the outer loop Loop structure is:The extract recovery tube with regulating valve is set between the first order funnel upper box part and separating box of infuser Road, separating box bottom and infuser first order top return jet pipe between set methanol eddy pipeline, and recovery pipe and return Flow tube is equipped with circulating pump on road.Rectifying loop is set between methanol eddy pipeline and mother liquor case, and the rectifying loop is by rectifying Regulating valve, rectifying column, condenser composition.Condenser is connected with mother liquor case.Set between mother liquor pipe and Sprayer Circulation pipe at different levels female Liquid regulating valve.
Two-stage is set inside described separating box casing is divided into three parts with the unconnected vertical baffle in top, extract is returned Line end is received in Part I, the initiating terminal of methanol eddy pipeline is in Part II, and overfall, recovery port are in Part III. First order dividing plate is higher than second level dividing plate, and sets separating tube on first order dividing plate.The end of recovery pipe in separating box Buffer cap is set.
Using the circulation dephenolizing process of circulation dephenolize device as described above, including extraction, methanol dephenolize, methanol time Receive and utilize.Described Methanol Recovery is got using being that the dephenolize methanol solution come out from infuser passes through precipitation separating box point liquid Top organic solution return to extraction workshop section, and the methanol mixed liquor containing phenol of a bottom part returns to the first of extracting and dephenolizing workshop section Level is recycled, and another part obtains liquid methanol after rectifying dephenolize is condensed again, is returned to methanol mother liquor case and is recycled.
After device as above and technique, methanol dephenolize solution is not only recycled in extraction sections at different levels, and it is mixed Liquid is closed because compositional concentration gradient difference between funnel cases at different levels so that form the reflux opposite with material direct of travel, to first The top of level funnel case is exported.Mixed liquor is separated in settling tank, and obtained top organic solution returns to extraction workshop section, bottom Supply dephenolizing extractor is directly returned to containing a phenol solution part, another part returns to methanol mother liquor after rectifying removes gossypol Case.
The loop that the invention has been constructed between precipitation separating box and dephenolizing extractor so that removed after precipitation separation organic molten The methanol solution containing phenol of agent directly returns to extraction dephenolize, is recycled.Simplify the technique that Methanol Recovery purification is recycled Link, shortens process route.Make process equipment compacter, save Methanol Recovery energy consumption, reduce the damage in Methanol Recovery stage Lose, reduce cost.
Brief description of the drawings
Fig. 1 is extraction production cottonseed protein circulation dephenolize apparatus structure schematic diagram of the present invention.
Fig. 2 is extraction production cottonseed protein circulation dephenolizing process flow chart of the present invention.
Embodiment
Such as Fig. 1 and Fig. 2, extraction cottonseed protein circulation dephenolize device, including multi-stage spray extraction infuser 1, separating box 2nd, rectifying column 9, condenser 19, methanol mother liquor case 3 and mother liquor pipe 13.Every grade of spraying and extracting, which leaches unit, includes shower 12, bottom Sieve tray disk 21, funnel case 5, Sprayer Circulation pump 16 and Sprayer Circulation pipe 15.The top of funnel case 5 connections at different levels, and according to material row Enter direction edge to raise step by step.Mother liquor pipe 13 is respectively connected with leading to Sprayer Circulation pipes 15 at different levels.
External circulation is constituted between described infuser 1 and separating box 2, the external circulation structure is:In leaching Go out between the top of first order funnel case 5 of device 1 and separating box 2 and set under the extract recovery pipe 6 with regulating valve 8, separating box 2 Methanol eddy pipeline 22, and recovery pipe 6 and return line are set between portion and time jet pipe 11 on the first order top of infuser 1 Circulating pump 26 is equipped with 22.
Rectifying loop is set between methanol eddy pipeline 22 and mother liquor case 3, and the rectifying loop is by rectifying regulating valve 7, essence Evaporate tower 9, condenser 19 to constitute, condenser 19 is connected with mother liquor case 3.Set between mother liquor pipe 13 and Sprayer Circulation pipe 15 at different levels female Liquid regulating valve 14.
The separating box 2 is that two-stage and top unconnected vertical baffle 4a, 4b are set inside precipitating type, separating box 2 by case Body is divided into three parts.The end of extract recovery pipe 6 is in Part I, and the initiating terminal of methanol eddy pipeline 22 is in Part II Bottom, overfall 17, recovery port 1 are located at the upper and lower part of Part III respectively.First order dividing plate 4a is higher than second level dividing plate 4b, and set separating tube 10 on first order dividing plate 4a.Mixed liquor into casing is obtained stable and tentatively sunk in Part I Form sediment and be layered, the organic solution on top climbs over dividing plate 4a into casing Part II, and separating tube 10 imports the methanol solution of bottom The middle part of Part II.Mixed liquor further precipitates separation in Part II, and the organic solution on top climbs over dividing plate 4b and enters Three parts, the phenol solution that contains of bottom enters return line 22.In Part III further precipitation separation after organic solution from overflow Head piece 17, which is collected, directly to be returned in the extraction workshop section before dephenolize, and the methanol solution of bottom deposition is temporary and is reaching finite concentration Afterwards rectifying loop is given from the pump of recovery port 1.The end of recovery tube 6 in the Part I of separating box 2 sets buffer cap 20, can make liquid Mutually stablize as early as possible.
Material right-to-left on bottom sieve pallet 21 is advanced in way step by step, is sprayed step by step in spray units at different levels.Thing Gossypol in material is reduced step by step, containing organic solvent, gossypol methyl alcohol mixed liquor because compositional concentration gradient difference is so as to each The reflux opposite with material direct of travel is formed between level funnel case 5, the top to first order funnel case 5 is exported.Mix afterwards Close liquid to separate in settling tank 2, obtained top organic solution returns to extraction workshop section, the phenol solution part that contains of bottom is directly returned Dephenolizing extractor 1 is supplied, another part returns to methanol mother liquor case 3 after rectifying loop removes gossypol.
It can control to reclaim the ratio of flow and circulation dephenolize flows at different levels using the regulating valve 8 in extract recovery pipe 6 Example.Similarly, it can control to enter rectifying loop using rectifying regulating valve 7 and be directly entered the flow containing phenol solution of digester 1 Both ratios are about 1 in ratio, the present embodiment:3.Again similarly, extraction dephenolize lists at different levels can be controlled using mother liquor regulating valve 14 The supply ratio of methanol mother liquor and circulation solution in the circulation pipe 15 of member, and alternation step by step, are specifically supplied with mother liquor Ratio decline step by step.
, can by increasing the flow of extraction mixed liquor recovery pipe 6, increasing the flow proportional containing phenol solution in rectifying loop So that the content of gossypol is constantly reduced in cottonseed protein.And due to the design in methanol loop loop so that the benefit of fresh methanol Reduced to consumption.Under the premise of cottonseed protein free phenol≤400ppm is reached, dephenolize workshop section saves energy consumption 30%, saves methanol 10% More than.Protein content >=50% in the cotton protein produced, organic solvent≤500ppm, methanol≤800ppm.

Claims (3)

1. a kind of extraction cottonseed protein circulates dephenolize device, including multi-stage spray extraction infuser(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, which leaches unit, includes shower (12), bottom sieve pallet(21), funnel case(5), Sprayer Circulation pump(16)And Sprayer Circulation pipe(15);Funnel cases at different levels(5)Top Connection, and raised step by step according to material direct of travel edge, mother liquor pipe(13)With Sprayer Circulation pipes at different levels(15)It is respectively connected with leading to; The separating box(2)For precipitating type, in separating box(2)The top of end sets overfall(17), bottom set the recovery with gate valve Mouthful(18);The dephenolize device is characterised by:
A. described infuser(1)With separating box(2)Between constitute external circulation, the external circulation structure is: Infuser(1)First order funnel case(5)Top and separating box(2)Between set with regulating valve(8)Extraction mixed liquor reclaim Pipeline(6), separating box(2)Bottom and infuser(1)Time jet pipe on first order top(11)Between set the pipe of methanol eddy containing phenol Road(22), and recovery pipe(6)And return line(22)On be equipped with circulating pump(26);
B. in methanol eddy pipeline(22)With mother liquor case(3)Between rectifying loop is set, the rectifying loop is by rectifying regulating valve (7), rectifying column(9), condenser(19)Composition, condenser(19)With mother liquor case(3)It is connected;
C. mother liquor pipe(13)With Sprayer Circulation pipes at different levels(15)Between set mother liquor regulating valve(14).
2. dephenolize device is circulated as claimed in claim 1, it is characterised in that described separating box(2)Inside sets two-stage and top Unconnected vertical baffle(4a、4b)Casing is divided into three parts, above-mentioned extraction mixed liquor recovery pipe(6)End is first Part, the pipeline of methanol eddy containing phenol(22)Initiating terminal in Part II, overfall(17), recovery port(18)In Part III; First order dividing plate(4a)Higher than second level dividing plate(4b), and in first order dividing plate(4a)On set separating tube(10);In separating box (2)Interior recovery pipe(6)End set buffer cap(20).
3. a kind of method for applying circulation dephenolize device as claimed in claim 1 or 2, including extraction, methanol dephenolize, first Alcohol is recycled, it is characterised in that described Methanol Recovery utilizes the methanol mixed solution for being to come out from infuser to divide by precipitation Liquid case point liquid, organic extraction workshop section before the top organic solution return dephenolize got, and the methyl alcohol mixed liquor containing phenol of bottom one The first order that part returns to extracting and dephenolizing workshop section is recycled, and another part obtains liquid first after rectifying dephenolize is condensed again Alcohol, returns to methanol mother liquor case and recycles.
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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CN107232387A (en) * 2016-07-18 2017-10-10 湖南欣瑞生物科技有限公司 A kind of extracting method of cottonseed protein

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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 examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2003252766A1 (en) * 2003-03-12 2004-09-30 Gao Shen Sdn. Bhd. Integrated process for separation of oil, protein, carbohydrates, shell and minor toxic components from seeds

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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Inventor after: Lu Zuowen

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Inventor before: Ge Yumei

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