CN104496802B - A kind of esterifying reaction method and esterification device of producing fatty acid triglycercide - Google Patents
A kind of esterifying reaction method and esterification device of producing fatty acid triglycercide Download PDFInfo
- Publication number
- CN104496802B CN104496802B CN201410707822.3A CN201410707822A CN104496802B CN 104496802 B CN104496802 B CN 104496802B CN 201410707822 A CN201410707822 A CN 201410707822A CN 104496802 B CN104496802 B CN 104496802B
- Authority
- CN
- China
- Prior art keywords
- esterifying
- esterifying kettle
- fatty acid
- aliphatic acid
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
- B01J2219/00763—Baffles
- B01J2219/00765—Baffles attached to the reactor wall
- B01J2219/00777—Baffles attached to the reactor wall horizontal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/19—Details relating to the geometry of the reactor
- B01J2219/192—Details relating to the geometry of the reactor polygonal
- B01J2219/1923—Details relating to the geometry of the reactor polygonal square or square-derived
- B01J2219/1925—Details relating to the geometry of the reactor polygonal square or square-derived prismatic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of esterifying reaction method and esterification device of producing fatty acid triglycercide. The method that object is to provide and device should have the feature that reaction efficiency is high, the reaction time is short, can produce high-load fatty acid triglycercide. Technical scheme is: a kind of esterifying reaction method of producing fatty acid triglycercide, carry out according to the following steps; 1) catalyst and glycerine carry out esterification; 2) control reaction pressure and the temperature in esterifying kettle; 3) export product by discharging opening. An esterification device of producing fatty acid triglycercide, comprises esterifying kettle; This reaction unit also comprises premixed still, aliphatic acid pre-heater; Premixed still is communicated with catalyst feeds and glycerine feed mouth, and the outlet of premixed still is communicated with atomizer; The intracavity bottom of esterifying kettle is provided with bubbling air sifter, and aliphatic acid pre-heater is communicated with aliphatic acid charging aperture; Aliphatic acid cooler and vacuum plant interface are also connected in esterifying kettle top, and the bottom of esterifying kettle also makes a discharging opening.
Description
Technical field
The present invention relates to a kind of method and apparatus of producing grease, particularly a kind of fatty acid glycerine three of producingThe esterifying reaction method of ester and esterification device.
Technical background
Aliphatic acid is to react for the production of classics edible, iundustrial oil with the esterification of glycerine. I.e. fatAcid generates monoglyceride with glycerine reaction, and monoglyceride and fatty acid response form two sweet esters, and two sweet esters are again with single sweetEster reaction forms triglycerides; As shown in the formula expression:
Traditional esterification device is stirring-type reactor, and the reactive mode also liquid-liquid that is confined to is reacted more,Its ubiquitous problem is: reaction esterification is incomplete, and monoglyceride in product, two sweet ester contents are higher,Adopt conventional method be difficult to directly acquisition highly purified fatty acid triglycercide, in the market more than 99%High-purity fatty acid triglycercide how purify through other means such as molecular clocks, not only complex process,And cost is higher.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned background technology, a kind of fatty acid triglycercide of producing is providedEsterifying reaction method and esterification device, the method and device should have that reaction efficiency is high, the reaction time is short,Can produce the feature of high-load fatty acid triglycercide, and described apparatus structure simple and stable, it is safe and reliable,Failure rate is low, easy to operate.
Technical scheme provided by the invention is:
Produce an esterifying reaction method for fatty acid triglycercide, carry out according to the following steps;
1) enter premixed still from catalyst and the glycerine of catalyst feeds and the input of glycerine feed mouth respectivelyMix, then input the inner chamber of esterifying kettle with the form of mist;
Meanwhile, from the aliphatic acid of aliphatic acid charging aperture input, after aliphatic acid pre-heater heating and gasifying from esterThe inner chamber of changing the bottom input esterifying kettle of still, carries out esterification with catalyst and glycerine;
2) aliphatic acid cooler and vacuum plant are connected the top of esterifying kettle, to the reaction pressure in esterifying kettleControl with temperature;
3) reactant that esterification generates sequentially down flows through the sieve plate of esterifying kettle inner chamber, then by esterificationThe discharging opening output product of still bottom.
The inner chamber bottom of described esterifying kettle is also provided with bubbling air sifter, after aliphatic acid gasification, inputs by bubbling air sifterEsterifying kettle inner chamber.
Described reaction temperature is 150-300 DEG C.
Described reaction pressure is 0.09-0.103323Mpa.
The time of described esterification is 40-120min.
An esterification device of producing fatty acid triglycercide, comprises esterifying kettle; It is characterized in that this reactionDevice also comprises premixed still, aliphatic acid pre-heater; Described premixed still be communicated with catalyst feeds andGlycerine feed mouth, the outlet of premixed still is by the atomizer of pipeline communication esterifying kettle inner chamber, to input aerosolThe catalyst of shape and glycerine; The intracavity bottom of described esterifying kettle is provided with bubbling air sifter, described aliphatic acidPre-heater is communicated with aliphatic acid charging aperture, and the outlet of aliphatic acid pre-heater is also by the drum described in pipeline communicationBubble air sifter, to input the fatty acid ester of gasification; It is cooling that aliphatic acid is also sequentially connected by pipeline in esterifying kettle topDevice and vacuum plant interface, the bottom of esterifying kettle also makes a discharging opening.
The cavity arrangements of described esterifying kettle has some sieve plates.
Operation principle of the present invention is: due to SCFA, medium chain fatty acid and middle LCFA boiling pointLow (boiling point≤300 DEG C), thereby can realize heat up gasification aliphatic acid and glycerine and carry out gas-liquid two phase reaction.For this reason, first by spraying into kettle after catalyst and the atomization of glycerine premixed gas, direct with the aliphatic acid gas in stillReact, at the bottom of the glyceride of formation and unreacted glycerine flow to still by sieve plate, way in also can with gasificationAliphatic acid carry out secondary esterification, the sustainable bubbling of bubbling air sifter of bottom of device, sinks to the thing at the bottom of stillMaterial carries out esterification for the third time with aliphatic acid bubble, can greatly improve reaction rate and product yield.
The invention has the beneficial effects as follows:
(1) compared with traditional reaction kettle of the esterification, gas liquid reaction efficiency is high, and the reaction time is short, is conducive to produceThe fatty acid triglycercide of high-load;
(2) device adopts atomized feed, and in still, increases sieve plate, and bottom bubbling can greatly improveReaction efficiency, package unit simple and stable, safe and reliable, failure rate is low, fitting operation is convenient, and cost is low,Applicable material is in extensive range.
Brief description of the drawings
Fig. 1 is the structural representation of esterification device of the present invention.
Number in the figure: 1-catalyst feeds; 2-glycerine feed mouth; 3-aliphatic acid charging aperture; 4-pre-Mixing kettle; 5-esterifying kettle; 6-atomizer; 7-sieve plate; 8-bubbling air sifter; 9-aliphatic acid pre-heater;10-aliphatic acid cooler; 11-discharging opening, 12-vacuum plant interface.
Detailed description of the invention
Aliphatic acid in triglycerides refers to single carbon chain fatty acid more, and than other aliphatic acid, its boiling point is lower,And when in the certain situation of aliphatic acid saturation degree, its boiling point reduces gradually along with the reduction of carbon chain lengths, spyBe not SCFA (as formic acid, acetic acid, propionic acid, butyric acid, acid), medium chain fatty acid (as sad,Capric acid) and the aliphatic acid (as laurate) of middle long carbochain, such aliphatic acid boiling point is many (to be shown 300 DEG C below1), and esterification reaction temperature mostly is 200-300 DEG C, therefore, adopts aliphatic acid (gas phase) and glycerine (liquidPhase) esterification technology, by improving esterification device, can improve the efficiency of esterification, obtainObtain highly purified triglycerides.
The different aliphatic acid of table 1 and boiling point thereof
The esterification device of production fatty acid triglycercide provided by the invention, comprises esterifying kettle 5, premixedStill 4, aliphatic acid pre-heater 9. Described premixed still is by pipeline communication catalyst feeds 1 and glycerineCharging aperture 2 mixes the catalyst of input and glycerine, then input esterifying kettle after output, and in esterifying kettleChamber sprays catalyst and glycerol mixture by atomizer 6 (being shower nozzle) with mist. And described fatAcid pre-heater is communicated with aliphatic acid charging aperture 3, the aliphatic acid of input is heated into after gaseous state, in esterifying kettleThe bubbling air sifter 8 of bottom, chamber is inputted esterifying kettle, makes the aliphatic acid of gaseous state and the catalyst of mist and glycerineReact; Aliphatic acid cooler and vacuum plant interface are also sequentially connected by pipeline in esterifying kettle top,Controlled reaction temperature (the inhibitory reaction generation of esterifying kettle inner chamber by aliphatic acid cooler (conventional freezing machinery)Temperature rise), and controlled the vacuum pressure of esterifying kettle inner chamber by vacuum plant (conventional air extractor). ReactionLiquid glycerin three esters that generate are exported by the discharging opening of esterifying kettle bottom.
As recommendation, the inner chamber of described esterifying kettle is also furnished with the sieve plate 7 of some (being generally 5-15 sheet).Sieve plate is arranged the arranged crosswise mode of recommend adoption routine.
The equal buyable of premixed still of the present invention, esterifying kettle, sieve plate and bubbling air sifter obtains.
Embodiment 1
Acetic acid (117 DEG C of boiling points) mixed acid is entered to esterifying kettle from bottom after the gasification of aliphatic acid pre-heater,Make acetic acid gas be full of still chamber, temperature in the kettle is controlled at 150 DEG C, then by catalyst and glycerine at premixed stillAfter middle stirring 30min, go out from still top spray by atomizer, carry out synthesis under normal pressure with the acetic acid gas in still,Reaction time 40min, continues logical acetic acid gas in course of reaction, after reaction finishes, stop logical acetic acid gas,Reactant is by discharge hole for discharge. Product after esterification is colourless transparent oil liquid, acid number (mgKOH/g)Be 0.09, triacetic acid content of triglyceride 99.5%.
Embodiment 2
Sad, capric acid mixed acid (238 DEG C of sad boiling points, 270 DEG C of capric acid boiling points) are added in advance through aliphatic acidAfter hot device gasification, enter esterifying kettle from bottom, make mixed acid gas be full of still chamber, temperature in the kettle is controlled at 275-280 DEG C, then catalyst and glycerine are stirred after 30min in premixed still, push up from still by atomizerEjection, carries out synthesis under normal pressure with the mixed acid gas in still, and reaction time 1h continues logical mixed in course of reactionClose acid gas, ensure that acid is slightly excessive, after reaction finishes, stop logical mixed acid gas, continue reaction 1h, anti-Answer thing by discharge hole for discharge. Product after esterification is colourless transparent oil liquid, and acid number (mgKOH/g) is0.06, pungent Triglyceride DDD content 99.2%.
Embodiment 3
Laurate (299 DEG C of boiling points) mixed acid is entered to esterification from bottom after the gasification of aliphatic acid pre-heaterStill, makes laurate gas be full of still chamber, and temperature in the kettle is controlled at 300 DEG C, and vacuum interface connects vacuum plant, protectsControlled underbalance (0.09Mpa) in card still. Catalyst and glycerine are stirred after 30min in premixed still, pass throughAtomizer goes out from still top spray, reacts with the laurate gas in still, and reaction time 1h, in course of reactionContinue logical laurate gas, after reaction finishes, stop logical laurate gas, continue reaction 1h, reactant byDischarge hole for discharge. The solid that is white in color after product after esterification is cooling, acid number (mgKOH/g) is 0.08, monthCinnamic acid content of triglyceride 98.6%.
Claims (7)
1. produce an esterifying reaction method for fatty acid triglycercide, carry out according to the following steps;
1) enter premixed still from the catalyst of catalyst feeds and glycerine feed mouth input and glycerine respectively and mix, then with the inner chamber of the form input esterifying kettle of mist;
Meanwhile, from the aliphatic acid of aliphatic acid charging aperture input, after aliphatic acid pre-heater heating and gasifying, input the inner chamber of esterifying kettle from the bottom of esterifying kettle, carry out esterification with catalyst and glycerine;
2) aliphatic acid cooler and vacuum plant are connected the top of esterifying kettle, and the reaction pressure in esterifying kettle and temperature are controlled;
3) reactant that esterification generates sequentially down flows through the sieve plate of esterifying kettle inner chamber, then by the discharging opening output product of esterifying kettle bottom.
2. the esterifying reaction method of production fatty acid triglycercide according to claim 1, is characterized in that the inner chamber bottom of described esterifying kettle is also provided with bubbling air sifter, after aliphatic acid gasification, inputs esterifying kettle inner chamber by bubbling air sifter.
3. the esterifying reaction method of production fatty acid triglycercide according to claim 2, is characterized in that described reaction temperature is 150-300 DEG C.
4. the esterifying reaction method of production fatty acid triglycercide according to claim 3, is characterized in that described reaction pressure is 0.09-0.103323Mpa.
5. the esterifying reaction method of production fatty acid triglycercide according to claim 4, the time that it is characterized in that described esterification is 40-120min..
6. produce an esterification device for fatty acid triglycercide, comprise esterifying kettle (5); It is characterized in that this reaction unit also comprises premixed still (4), aliphatic acid pre-heater (9); Described premixed still is communicated with catalyst feeds (1) and glycerine feed mouth (2), and the outlet of premixed still is by the atomizer (6) of pipeline communication esterifying kettle inner chamber, to input catalyst and the glycerine of mist; The intracavity bottom of described esterifying kettle is provided with bubbling air sifter (8), described aliphatic acid pre-heater is communicated with aliphatic acid charging aperture (3), the outlet of aliphatic acid pre-heater is also by the bubbling air sifter described in pipeline communication, to input the fatty acid ester of gasification; Aliphatic acid cooler (10) and vacuum plant interface (12) are also sequentially connected by pipeline in esterifying kettle top, and the bottom of esterifying kettle also makes a discharging opening.
7. the esterification device of production fatty acid triglycercide according to claim 6, is characterized in that the cavity arrangements of described esterifying kettle has the sieve plate (7) of some.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410707822.3A CN104496802B (en) | 2014-11-28 | 2014-11-28 | A kind of esterifying reaction method and esterification device of producing fatty acid triglycercide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410707822.3A CN104496802B (en) | 2014-11-28 | 2014-11-28 | A kind of esterifying reaction method and esterification device of producing fatty acid triglycercide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104496802A CN104496802A (en) | 2015-04-08 |
| CN104496802B true CN104496802B (en) | 2016-05-04 |
Family
ID=52938277
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410707822.3A Active CN104496802B (en) | 2014-11-28 | 2014-11-28 | A kind of esterifying reaction method and esterification device of producing fatty acid triglycercide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104496802B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111495276B (en) * | 2019-01-30 | 2022-09-23 | 宁波富理电池材料科技有限公司 | High-temperature high-pressure gas-solid reaction kettle |
| CN109836328A (en) * | 2019-03-16 | 2019-06-04 | 广州隽沐生物科技股份有限公司 | The synthetic method of median chain triglyceride oil |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2013319B1 (en) * | 2006-04-28 | 2019-01-23 | Sk Chemicals Co., Ltd. | Method for preparing fatty acid alkyl ester using fatty acid distillate |
| US8022236B2 (en) * | 2007-10-12 | 2011-09-20 | Aiken John E | Fatty acid alkyl ester production from oleaginous seeds |
| CN101305763B (en) * | 2008-06-10 | 2010-06-16 | 无锡市双惠化工有限公司 | Granulation method of granulating food additive rosin glyceride |
| CN101638610A (en) * | 2009-08-13 | 2010-02-03 | 铁岭北亚药用油有限公司 | Medicinal medium-chain triglyceride esterification reaction tank |
| CN102153465B (en) * | 2011-02-15 | 2013-08-28 | 浙江赞宇科技股份有限公司 | Method for preparing low acid-value fatty acid methyl ester |
| CN204281647U (en) * | 2014-11-28 | 2015-04-22 | 浙江赞宇科技股份有限公司 | A kind of esterification device producing fatty acid triglycercide |
-
2014
- 2014-11-28 CN CN201410707822.3A patent/CN104496802B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104496802A (en) | 2015-04-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101148409B (en) | Method for preparing fatty acid ester in microchannel reactor | |
| US20090038209A1 (en) | Method of Biodiesel Production | |
| CN104496802B (en) | A kind of esterifying reaction method and esterification device of producing fatty acid triglycercide | |
| CN101397504A (en) | Production process of biological diesel oil and apparatus | |
| CN104152275B (en) | A kind of gas-phase methanol esterification device | |
| CN103242966A (en) | Technology process for producing biodiesel and key preparation device | |
| CN204281647U (en) | A kind of esterification device producing fatty acid triglycercide | |
| CN101829528A (en) | Hydrolysis tower for oil and fat hydrolysis and method for oil hydrolysis by using same | |
| CN102586027A (en) | Continuous production method of biodiesel from waste oil/fat | |
| CN103087788B (en) | Method for preparing biodiesel by using high-acid value oil | |
| CN204841658U (en) | Gas phase reaction prepares biodiesel's device in succession | |
| CN100590176C (en) | Ester interchange method for producing bio-diesel oil | |
| CN204342761U (en) | A kind of device realizing continuous prodution triglyceride level | |
| CN201272776Y (en) | Apparatus for continuous preparation of biodiesel by neutral grease | |
| CN205412291U (en) | Biodiesel multistage atomization dealcoholize device | |
| CN203513650U (en) | Biodiesel production device | |
| CN201701927U (en) | Fatty acid methyl ester esterification reaction kettle | |
| CN203890322U (en) | Glycerolysis and esterification reaction device | |
| CN111411024A (en) | Method and device for producing biodiesel by micro-reaction ester exchange | |
| CN205275489U (en) | Produce separator of glycerine and methyl alcohol in biodiesel technology | |
| CN206173289U (en) | Adopt pressurization catalysis high acid value trench oil first esterified device in succession | |
| CN219886017U (en) | Energy-saving production device for preparing biodiesel | |
| CN105418369A (en) | Separating device and method for glycerinum and methyl alcohol produced in biodiesel technology | |
| CN203209050U (en) | Reaction and separation integrated cracker | |
| CN104830543A (en) | Device and method for preparing biodiesel through continuous gas-phase catalytic esterification |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Hangzhou City, Zhejiang province 310009 City Shangcheng District No. 128 Lane Patentee after: ZANYU TECHNOLOGY GROUP CO.,LTD. Patentee after: HANGZHOU OLEOCHEMICALS CO.,LTD. Address before: Hangzhou City, Zhejiang province 310009 City Shangcheng District No. 128 Lane Patentee before: ZHEJIANG ZANYU TECHNOLOGY Co.,Ltd. Patentee before: HANGZHOU OLEOCHEMICALS CO.,LTD. |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Hangzhou City, Zhejiang province 310009 City Shangcheng District No. 128 Lane Patentee after: ZANYU TECHNOLOGY GROUP CO.,LTD. Patentee after: Hangzhou Zanyu Oil Technology Co.,Ltd. Address before: Hangzhou City, Zhejiang province 310009 City Shangcheng District No. 128 Lane Patentee before: ZANYU TECHNOLOGY GROUP CO.,LTD. Patentee before: HANGZHOU OLEOCHEMICALS CO.,LTD. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231120 Address after: Room C706, No. 198 Qidi Road, Economic and Technological Development Zone, Xiaoshan District, Hangzhou City, Zhejiang Province, 310000 Patentee after: Hangzhou Zanyu Chemical Co.,Ltd. Address before: Hangzhou City, Zhejiang province 310009 City Shangcheng District No. 128 Lane Patentee before: ZANYU TECHNOLOGY GROUP CO.,LTD. Patentee before: Hangzhou Zanyu Oil Technology Co.,Ltd. |