CN104496802A - Esterification reaction method and device for production of fatty acid triglyceride - Google Patents
Esterification reaction method and device for production of fatty acid triglyceride Download PDFInfo
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- CN104496802A CN104496802A CN201410707822.3A CN201410707822A CN104496802A CN 104496802 A CN104496802 A CN 104496802A CN 201410707822 A CN201410707822 A CN 201410707822A CN 104496802 A CN104496802 A CN 104496802A
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- fatty acid
- esterifying kettle
- reaction
- esterifying
- esterification
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- 238000005886 esterification reaction Methods 0.000 title claims abstract description 38
- 239000000194 fatty acid Substances 0.000 title claims abstract description 37
- 235000014113 dietary fatty acids Nutrition 0.000 title claims abstract description 36
- 229930195729 fatty acid Natural products 0.000 title claims abstract description 36
- 150000004665 fatty acids Chemical class 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 title abstract description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 230000032050 esterification Effects 0.000 claims abstract description 31
- 235000011187 glycerol Nutrition 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 230000005587 bubbling Effects 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims description 52
- 150000002632 lipids Chemical class 0.000 claims description 38
- 238000002309 gasification Methods 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000003595 mist Substances 0.000 claims description 6
- 238000004891 communication Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- -1 fatty acid ester Chemical class 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 14
- 238000009835 boiling Methods 0.000 description 10
- 239000005639 Lauric acid Substances 0.000 description 7
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 150000002148 esters Chemical class 0.000 description 5
- OGBUMNBNEWYMNJ-UHFFFAOYSA-N batilol Chemical class CCCCCCCCCCCCCCCCCCOCC(O)CO OGBUMNBNEWYMNJ-UHFFFAOYSA-N 0.000 description 4
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 3
- 235000009508 confectionery Nutrition 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000004667 medium chain fatty acids Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 150000004666 short chain fatty acids Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 125000005908 glyceryl ester group Chemical group 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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 invention relates to an esterification reaction method and device for production of fatty acid triglyceride. The esterification reaction method and device for production of fatty acid triglyceride have the characteristics of high reaction efficiency and short reaction time and can be used for producing high-content fatty acid triglyceride. The esterification reaction method comprises the following steps: (1) carrying out esterification reaction on a catalyst and glycerin; (2) controlling the reaction pressure and the reaction temperature in an esterification reactor; and (3) discharging the product of reaction through a discharge port. The esterification reaction device for production of fatty acid triglyceride comprises an esterification reactor and further comprises a pre-mixing tank and a fatty acid pre-heater, wherein the pre-mixing tank is communicated with a catalyst feed port and a glycerin feed port, the outlet of the pre-mixing tank is communicated with an atomizer, the bottom of the inner cavity of the esterification reactor is provided with a bubbling air sifter, the fatty acid pre-heater is communicated with a fatty acid feed port, the top of the esterification reactor is communicated with a fatty acid cooler and a vacuum device interface, and the bottom of the esterification reactor is provided with a discharge port.
Description
Technical field
The present invention relates to a kind of method and apparatus producing grease, particularly a kind of esterifying reaction method and esterification device producing fatty acid triglycercide.
Technical background
The esterification of lipid acid and glycerine is reacted for the production of classics that are edible, technical oils.Namely lipid acid and glycerine reaction generate mono-glycerides, and mono-glycerides and fatty acid response form two sweet esters, and two sweet esters react with mono-glycerides and form triglyceride level; As shown in the formula expression:
Traditional esterification device is stirring-type reactor, reactive mode also more is confined to liquid-liquid reaction, its ubiquitous problem is: reaction esterification is incomplete, mono-glycerides in product, two sweet ester contents are higher, traditional method is adopted to be difficult to directly obtain highly purified fatty acid triglycercide, high-purity fatty acid triglycercide of in the market more than 99% is many purifies through other means such as molecular distillations, not only complex process, and cost is higher.
Summary of the invention
The object of the invention is the deficiency overcoming above-mentioned background technology, a kind of esterifying reaction method and the esterification device of producing fatty acid triglycercide are provided, the method and device should have the feature that reaction efficiency is high, the reaction times is short, can produce high-content fatty acid triglycercide, and described apparatus structure simple and stable, 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 pre-mixing still and mix from the catalyzer of catalyst feeds and the input of glycerine feed mouth and glycerine, then with the inner chamber of the form of mist input esterifying kettle respectively;
Meanwhile, from the lipid acid of fatty acid feedstock mouth input, from the inner chamber of the bottom input esterifying kettle of esterifying kettle after lipid acid pre-heaters heating and gasifying, carry out esterification with catalyzer and glycerine;
2) top of esterifying kettle connected by lipid acid water cooler and vacuum unit, controls the reaction pressure in esterifying kettle and temperature;
3) reactant that esterification generates sequentially down flows through the sieve plate of esterifying kettle inner chamber, then exports product by the discharge port of esterifying kettle bottom.
The inner chamber bottom of described esterifying kettle is also provided with bubbling air sifter, by bubbling air sifter input esterifying kettle inner chamber after lipid acid gasification.
Described temperature of reaction is 150-300 DEG C.
Described reaction pressure is 0.09-0.103323Mpa.
The time of described esterification is 40-120min.
Produce an esterification device for fatty acid triglycercide, comprise esterifying kettle; It is characterized in that this reaction unit also comprises pre-mixing still, lipid acid pre-heaters; Described pre-mixing still is communicated with catalyst feeds and glycerine feed mouth, the outlet of pre-mixing still by the spraying gun of pipeline communication esterifying kettle inner chamber, to input catalyzer and the glycerine of mist; The intracavity bottom of described esterifying kettle is provided with bubbling air sifter, and described lipid acid pre-heaters is communicated with fatty acid feedstock mouth, and the bubbling air sifter described in pipeline communication is also passed through in the outlet of lipid acid pre-heaters, to input the fatty acid ester of gasification; Lipid acid water cooler and vacuum unit interface are also sequentially connected by pipeline in esterifying kettle top, and the bottom of esterifying kettle also makes a discharge port.
The cavity arrangements of described esterifying kettle has some amount sieve plate.
Principle of work of the present invention is: due to short chain fatty acid, medium chain fatty acid and middle longer chain fatty acid boiling point lower (boiling point≤300 DEG C), thus can realize heat up gasification lipid acid and glycerine carry out gas-liquid two phase reaction.For this reason, kettle is sprayed into after first catalyzer and glycerine premixed gas being atomized, directly react with the lipid acid gas in still, the glyceryl ester formed and unreacted glycerine flow at the bottom of still by sieve plate, also secondary esterification can be carried out with the lipid acid of gasification in way, the sustainable bubbling of bubbling air sifter of bottom of device, sinks to material at the bottom of still and lipid acid bubble carries out third time esterification, greatly can improve speed of reaction and product yield.
The invention has the beneficial effects as follows:
(1) compared with traditional esterifications reactor, gas liquid reaction efficiency is high, and the reaction times is short, is conducive to the fatty acid triglycercide producing high-content;
(2) device adopts atomized feed, and increases sieve plate in still, and bottom bubbling greatly can improve reaction efficiency, complete assembly simple and stable, safe and reliable, failure rate is low, and install easy to operate, cost is low, and the material be suitable for is in extensive range.
Accompanying drawing explanation
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-fatty acid feedstock mouth; 4-pre-mixing still; 5-esterifying kettle; 6-spraying gun; 7-sieve plate; 8-bubbling air sifter; 9-lipid acid pre-heaters; 10-lipid acid water cooler; 11-discharge port, 12-vacuum unit interface.
Embodiment
The single chain fatty acid of the many fingers of lipid acid in triglyceride level, compared to other lipid acid, its boiling point is lower, and when lipid acid saturation ratio is certain, its boiling point reduces gradually along with the reduction of carbon chain lengths, particularly short chain fatty acid is (as formic acid, acetic acid, propionic acid, butyric acid, acid), medium chain fatty acid is (as sad, capric acid) and the lipid acid (as lauric acid) of middle Long carbon chain, such lipid acid boiling point is many below 300 DEG C (table 1), and esterification reaction temperature mostly is 200-300 DEG C, therefore, adopt the esterification technology of lipid acid (gas phase) and glycerine (liquid phase), by improving esterification device, the efficiency of esterification can be improved, obtain highly purified triglyceride level.
The different lipid acid of table 1 and boiling point thereof
The esterification device of production fatty acid triglycercide provided by the invention, comprises esterifying kettle 5, pre-mixing still 4, lipid acid pre-heaters 9.The catalyzer of input and glycerine are mixed by pipeline communication catalyst feeds 1 and glycerine feed mouth 2 by described pre-mixing still, then input esterifying kettle after exporting, and by spraying gun 6 (i.e. shower nozzle), catalyzer and glycerol mixture are sprayed with mist at esterifying kettle inner chamber.And described lipid acid pre-heaters is communicated with fatty acid feedstock mouth 3, after the lipid acid of input is heated into gaseous state, inputs esterifying kettle by the bubbling air sifter 8 of esterifying kettle intracavity bottom, the lipid acid of gaseous state and the catalyzer of mist and glycerine are reacted; Lipid acid water cooler and vacuum unit interface are also sequentially connected by pipeline in esterifying kettle top, controlled the temperature of reaction (temperature rise that inhibited reaction produces) of esterifying kettle inner chamber by lipid acid water cooler (conventional freezing machinery), and controlled the vacuum pressure of esterifying kettle inner chamber by vacuum unit (conventional air extractor).Liquid glycerin three ester that reaction generates then is exported by the discharge port of esterifying kettle bottom.
As recommendation, the inner chamber of described esterifying kettle is also furnished with the sieve plate 7 of some amount (being generally 5-15 sheet).Sieve plate is arranged and is recommended to adopt conventional arranged crosswise mode.
The equal buyable of pre-mixing still of the present invention, esterifying kettle, sieve plate and bubbling air sifter obtains.
Embodiment 1
Acetic acid (boiling point 117 DEG C) mixing acid is entered esterifying kettle from bottom after the gasification of lipid acid pre-heaters, acetic acid gas is made to be full of still chamber, temperature in the kettle controls at 150 DEG C, after then catalyzer and glycerine being stirred 30min in pre-mixing still, is gone out from still top spray by spraying gun, synthesis under normal pressure is carried out with the acetic acid gas in still, reaction times 40min, continues logical acetic acid gas, after reaction terminates in reaction process, stop logical acetic acid gas, reactant is by discharge hole for discharge.Product after esterification is colourless transparent oil liquid, and acid number (mg KOH/g) is 0.09, nitrilotriacetic content of triglyceride 99.5%.
Embodiment 2
By sad, capric acid mixing acid (sad boiling point 238 DEG C, capric acid boiling point 270 DEG C) after the gasification of lipid acid pre-heaters, enter esterifying kettle from bottom, mixing acid gas is made to be full of still chamber, temperature in the kettle controls at 275-280 DEG C, then after catalyzer and glycerine being stirred 30min in pre-mixing still, gone out from still top spray by spraying gun, synthesis under normal pressure is carried out with the mixing acid gas in still, reaction times 1h, logical mixing acid gas is continued in reaction process, ensure the acid amount of skipping over, after reaction terminates, stop logical mixing acid gas, continue reaction 1h, reactant is by discharge hole for discharge.Product after esterification is colourless transparent oil liquid, and acid number (mg KOH/g) is 0.06, pungent Triglyceride DDD content 99.2%.
Embodiment 3
Lauric acid (boiling point 299 DEG C) mixing acid is entered esterifying kettle from bottom after the gasification of lipid acid pre-heaters, lauric acid gas is made to be full of still chamber, temperature in the kettle controls at 300 DEG C, and vacuum interface connects vacuum unit, ensures controlled underbalance (0.09Mpa) in still.After catalyzer and glycerine are stirred 30min in pre-mixing still, gone out from still top spray by spraying gun, react with the lauric acid gas in still, reaction times 1h, continue logical lauric acid gas in reaction process, after reaction terminates, stop logical lauric acid gas, continue reaction 1h, reactant is by discharge hole for discharge.In white solid after product cooling after esterification, acid number (mg KOH/g) is 0.08, lauric acid three ester content 98.6%.
Claims (7)
1. produce an esterifying reaction method for fatty acid triglycercide, carry out according to the following steps;
1) enter pre-mixing still and mix from the catalyzer of catalyst feeds and the input of glycerine feed mouth and glycerine, then with the inner chamber of the form of mist input esterifying kettle respectively;
Meanwhile, from the lipid acid of fatty acid feedstock mouth input, from the inner chamber of the bottom input esterifying kettle of esterifying kettle after lipid acid pre-heaters heating and gasifying, carry out esterification with catalyzer and glycerine;
2) top of esterifying kettle connected by lipid acid water cooler and vacuum unit, controls the reaction pressure in esterifying kettle and temperature;
3) reactant that esterification generates sequentially down flows through the sieve plate of esterifying kettle inner chamber, then exports product by the discharge port 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, by bubbling air sifter input esterifying kettle inner chamber after lipid acid gasification.
3. the esterifying reaction method of production fatty acid triglycercide according to claim 2, is characterized in that described temperature of reaction 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, is characterized in that the time of 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 pre-mixing still (4), lipid acid pre-heaters (9); Described pre-mixing still is communicated with catalyst feeds (1) and glycerine feed mouth (2), the outlet of pre-mixing still by the spraying gun (6) of pipeline communication esterifying kettle inner chamber, to input catalyzer and the glycerine of mist; The intracavity bottom of described esterifying kettle is provided with bubbling air sifter (8), described lipid acid pre-heaters is communicated with fatty acid feedstock mouth (3), the bubbling air sifter described in pipeline communication is also passed through in the outlet of lipid acid pre-heaters, to input the fatty acid ester of gasification; Lipid acid water cooler (10) and vacuum unit interface (12) are also sequentially connected by pipeline in esterifying kettle top, and the bottom of esterifying kettle also makes a discharge port.
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 amount.
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| 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 |
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| CN201410707822.3A CN104496802B (en) | 2014-11-28 | 2014-11-28 | A kind of esterifying reaction method and esterification device of producing fatty acid triglycercide |
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| CN104496802A true CN104496802A (en) | 2015-04-08 |
| CN104496802B CN104496802B (en) | 2016-05-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN111495276A (en) * | 2019-01-30 | 2020-08-07 | 宁波富理电池材料科技有限公司 | High-temperature high-pressure gas-solid reaction kettle |
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| CN111495276A (en) * | 2019-01-30 | 2020-08-07 | 宁波富理电池材料科技有限公司 | High-temperature high-pressure gas-solid reaction kettle |
| 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 |
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|---|---|
| CN104496802B (en) | 2016-05-04 |
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