CN213102131U - System for preparing methyl myristate - Google Patents
System for preparing methyl myristate Download PDFInfo
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- CN213102131U CN213102131U CN202021065368.3U CN202021065368U CN213102131U CN 213102131 U CN213102131 U CN 213102131U CN 202021065368 U CN202021065368 U CN 202021065368U CN 213102131 U CN213102131 U CN 213102131U
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- ZAZKJZBWRNNLDS-UHFFFAOYSA-N methyl tetradecanoate Chemical compound CCCCCCCCCCCCCC(=O)OC ZAZKJZBWRNNLDS-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000003054 catalyst Substances 0.000 claims abstract description 112
- 239000011973 solid acid Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims description 37
- 238000000605 extraction Methods 0.000 claims description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 12
- 239000007791 liquid phase Substances 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000012264 purified product Substances 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 12
- 230000008676 import Effects 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 18
- 229920001429 chelating resin Polymers 0.000 description 17
- 238000005886 esterification reaction Methods 0.000 description 11
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 7
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 6
- 235000021360 Myristic acid Nutrition 0.000 description 6
- 239000003729 cation exchange resin Substances 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 238000003912 environmental pollution Methods 0.000 description 6
- 239000003377 acid catalyst Substances 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000007086 side reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000003225 biodiesel Substances 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000686 essence Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003930 superacid Substances 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The utility model provides a system for preparation methyl myristate. The system mixes the jar in advance including being used for with the raw materials carries out premixing, mix jar connection in advance and mix the cauldron entirely, be provided with the catalyst import that is used for letting in solid acid catalyst and the raw materials import that lets in the raw materials on mixing the cauldron entirely, be provided with temperature regulating device on mixing the cauldron entirely. The utility model discloses a system cost is low, operation method, utilize the yield height of the methyl myristate that this system obtained.
Description
Technical Field
The utility model relates to a preparation field of methyl myristate particularly, relates to a system for preparing methyl myristate.
Background
Due to exhaustion of conventional non-renewable diesel and increase of artificial emission of greenhouse gases, biodiesel is regarded as a promising alternative energy source and has received wide attention in recent years. Methyl myristate, as one of the main components of biodiesel, has the advantages of high cetane number, high flash point, good emission characteristics, reproducibility, excellent biodegradability and the like, and is considered as a diesel additive and a fuel substitute with great potential. Besides being used for biodiesel, the methyl myristate can also be used for edible essences such as honey, coconut and the like, and daily essences, and can also be used for preparing organic chemicals. Therefore, the methyl myristate serving as an important fatty acid methyl ester has great application value, and the development of a green and economic methyl myristate process route is of great practical significance.
At present, myristic acid and methanol are generally used as raw materials in industrial production of methyl myristate, concentrated sulfuric acid is used as a catalyst to carry out esterification reaction, and the concentrated sulfuric acid has quite high activity, but has the defects of serious equipment corrosion, difficulty in continuous production, strict acidity requirement, serious environmental pollution and the like, and is difficult to separate and purify products, more in byproducts and greatly reduced in yield.
In view of this, the present invention is especially provided.
SUMMERY OF THE UTILITY MODEL
The utility model has the first purpose of providing a preparation method of methyl myristate, this preparation method uses solid acid catalyst to replace liquid acid catalyst, and the specific surface area and the pore volume of solid acid catalyst are all bigger, have ensured good selectivity and reactivity, easily result separation and purification, and can use repeatedly many times, have avoided equipment corrosion and environmental pollution, make the enterprise can the continuity production; under the specific condition of the specific solid acid catalyst dosage, the reaction efficiency is greatly improved, the occurrence of side reactions is inhibited, the conversion rate of the product can reach 97.8-99.7%, and the yield of the final product methyl myristate is improved.
The second objective of the present invention is to provide a system using the above preparation method, which has the advantages of low cost, convenient operation, and high yield of methyl myristate obtained by using the system.
In order to realize the above purpose of the utility model, the following technical scheme is adopted:
the utility model provides a preparation method of methyl myristate, which comprises the following steps:
mixing and stirring the tetradecanoic acid and the methanol according to the molar ratio of 1 (2-6) to form a mixture, heating to 50-60 ℃, and adding a solid acid catalyst accounting for 10-30 wt% of the mixture for esterification reaction.
In the prior art, myristic acid and methanol are generally used as raw materials for industrially producing methyl myristate, concentrated sulfuric acid is used as a catalyst for esterification reaction, and the concentrated sulfuric acid has quite high activity, but has the defects of serious equipment corrosion, difficulty in continuous production, strict acidity requirement, serious environmental pollution and the like, and is difficult to separate and purify a product, more in byproducts and greatly reduced in yield.
The preparation method of the utility model uses the solid acid catalyst to replace the liquid acid catalyst, the specific surface area and the pore volume of the solid acid catalyst are both larger, thereby ensuring good selectivity and reaction activity, being easy to separate and purify the product, being capable of being used repeatedly, avoiding the corrosion of equipment and environmental pollution, and enabling enterprises to produce continuously; under the specific condition of the catalyst dosage of 10-30 wt% of the mixture, the reaction efficiency is greatly improved, the occurrence of side reaction is inhibited, the conversion rate of the product can reach 97.8% -99.7%, and the yield and the quality of the final product methyl myristate are greatly improved.
The utility model discloses an in the scheme, not only adopted solid acid catalyst to replace traditional liquid acid catalyst to optimize the quantity of the solid acid catalyst who adopts, because too big not only the subsequent processing increases the burden when the catalyst quantity, can not further increase the conversion rate of reaction yet, if the catalyst quantity plays due catalytic effect again too seldom, therefore suitable catalyst quantity is necessary.
Preferably, the amount of the solid acid catalyst is 15-25 wt% of the mass of the mixture; preferably, the solid acid catalyst is used in an amount of 20 wt%. The utility model discloses the people discovers through a large amount of practices, thereby solid acid catalyst's specific surface area is big so that the catalyst that load metal ion generated can obtain good dispersion, and the reactant can adsorb on the surface structure of cavity, and the catalyst concentration who makes to be in reaction center position because of reactant molecule and metal ion take place the reaction improves greatly to a great extent has improved reactivity, when the catalyst optimum amount is 20 wt%, the conversion rate of product has reached 99.7%.
Preferably, the solid acid catalyst is at least one of cation exchange resin and solid super acid; compared with other solid acid catalysts, the solid acid catalyst is cation exchange resin, and the cation exchange resin and the solid super acid have the characteristics of good stability, easy separation from reactants and repeated use, and particularly the cation exchange resin not only has excellent catalytic performance, but also has higher mechanical strength.
Preferably, the cation exchange resin is Amberlyst 39wet, Amberlyst 36wet or Amberlyst 35 wet. Preferably, the cation exchange resin is Amberlyst 39 wet. Amberlyst 39wet, Amberlyst 36wet or Amberlyst 35wet are ion exchange resin series produced by the Dow chemical method, especially Amberlyst 39wet is a macroporous strong acid low crosslinking degree catalyst, and the open pore structure is especially suitable for esterification reaction.
Preferably, the stirring speed is 400rpm-600rpm, the raw material conversion rate can be improved by controlling the proper stirring speed, and the produced methyl myristate has more excellent performance.
Preferably, after the esterification reaction, the method further comprises the step of performing quantitative analysis on a reaction product after the esterification reaction, wherein the quantitative analysis adopts a gas chromatograph;
preferably, the operating condition of the gas chromatograph is that the carrier gas is N2And column front pressure: 45.2 kPa; the tail blow (N2) flow rate was: 30 mL/min; h2: 40 mL/min; air: 400 mL/min; the temperature of the gasification chamber is 270-280 ℃, the temperature of the detector is 280-290 ℃, and the sample injection amount is 0.5 mu L. The gas chromatograph is adopted to carry out qualitative and quantitative analysis on the sample, and the esterification reaction process, the product quality and the yield can be quickly and accurately controlled and analyzed.
The utility model also provides an adopt preparation system of above-mentioned preparation method, including being used for carrying out the jar that mixes in advance with the raw materials, mix jar connection in advance and mix the cauldron entirely, mix the raw materials import that is provided with the catalyst import that is used for letting in solid acid catalyst and lets in the raw materials on the cauldron entirely, be provided with temperature regulating device on mixing the cauldron entirely.
Preferably, the side wall of the full mixing kettle is provided with a product outlet, and a reaction product enters the catalyst separator from the product outlet to separate and recover the catalyst;
preferably, a liquid phase outlet is arranged at the top of the catalyst separator, and a membrane filter is connected to the liquid phase outlet for separating the catalyst in the liquid phase material;
preferably, the bottom of the membrane filter is provided with a catalyst recovery port, the side wall of the membrane filter is provided with a product outlet for discharging purified products, and the catalyst recovery port is connected with the side wall of the catalyst separator for returning part of materials to the catalyst separator to continue purification and separation.
Preferably, the bottom of the full mixing kettle is provided with a first catalyst outlet; and a second catalyst outlet is arranged at the bottom of the catalyst separator, and the second catalyst outlet is communicated with the first catalyst outlet for common recovery.
Preferably, the system further comprises a catalyst regenerator, the side walls of which are connected with the first and second catalyst outlets, respectively; preferably, the side wall of the catalyst regenerator is connected to the catalyst inlet for the regenerated catalyst to be returned to the complete mixing tank.
Preferably, the product outlet is connected to a first rectification column for separating the product from methanol; and a tower top condenser is arranged at the tower top of the first rectifying tower, part of condensate coming out of the tower top condenser returns to the first rectifying tower, and part of condensate goes to the premixing tank.
Preferably, a heavy component outlet is formed in the bottom of the first rectifying tower, and the heavy component outlet is connected with an extraction tower for product extraction and purification.
Preferably, the top of the extraction tower is provided with an extraction solvent spray nozzle, the bottom of the extraction tower is provided with an extraction liquid outlet, and the extraction liquid outlet is connected with the second rectification tower to remove the extraction solvent.
Compared with the prior art, the beneficial effects of the utility model reside in that:
the preparation method of the utility model uses the solid acid catalyst to replace the liquid acid catalyst, the specific surface area and the pore volume of the solid acid catalyst are both larger, thereby ensuring good selectivity and reaction activity, being easy to separate and purify the product, being capable of being repeatedly used for many times, avoiding the corrosion of equipment and environmental pollution, and enabling enterprises to continuously produce; under the specific condition of the catalyst dosage of 10-30 wt% of the mixture, the reaction efficiency is greatly improved, the occurrence of side reaction is inhibited, the conversion rate of the product can reach 97.8% -99.7%, and the yield of the final product methyl myristate is improved.
The utility model discloses a preparation system is with low costs, convenient operation, utilize the yield height of the methyl myristate that this system obtained.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic structural diagram of a system for preparing methyl myristate according to an embodiment of the present invention;
FIG. 2 is a graph showing the effect of the amount of catalyst used in examples 1-5 on the esterification reaction of myristic acid;
FIG. 3 is a graph showing the effect of different catalysts on the esterification reaction of myristic acid in examples 6-9;
FIG. 4 is a gas chromatogram of the reaction product obtained in example 3 of the present invention;
fig. 5 is a gas chromatogram of the product obtained in example 10 of the present invention.
Description of the drawings:
1-a premixing tank; 2-a full mixing kettle;
21-raw material inlet; 22-catalyst inlet;
23-a product outlet; 24-a first catalyst outlet;
201-temperature control device;
3-a catalyst separator; 31-a liquid phase outlet;
301-a membrane filter; 3010-product outlet;
32-a second catalyst outlet; 4-a first rectification column;
401-overhead condenser; 42-heavy ends outlet;
5-an extraction column; 51-an extract outlet;
501-an extraction solvent spray head; 6-a second rectification column;
7-catalyst regenerator.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings and detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to clarify the technical solution of the present invention, the following description is made in the form of specific embodiments.
Example 1
Adopting the system shown in FIG. 1, introducing the myristic acid and methanol into a premixing tank 1 according to a molar ratio of 1:5, stirring at a speed of 400rpm-600rpm until the myristic acid is completely dissolved to form a mixture, and then feeding the mixture into a full mixing kettle 2 from a raw material inlet 21;
simultaneously, a catalyst Amberlyst 39wet accounting for 10 wt% of the mixture is added into the full mixing kettle 2 through a catalyst inlet 22 for esterification reaction, a temperature control device 201 is arranged on the full mixing kettle 2 and used for controlling the temperature in the esterification reaction process to be kept at 50-60 ℃, samples are taken at certain time intervals for gas chromatography analysis, and the operating condition of a gas chromatograph is that the carrier gas is N2And column front pressure: 45.2 kPa; tail blowing (N)2) The flow rate is as follows: 30 mL/min; h2: 40 mL/min; air: 400 mL/min; the temperature of the gasification chamber is 270-280 ℃, the temperature of the detector is 280-290 ℃, and the sample injection amount is 0.5 mu L.
The reaction product enters a catalyst separator 3 for catalyst separation after coming out from a product outlet 23, a liquid phase outlet 31 is arranged at the top of the catalyst separator 3, the liquid phase outlet 31 is connected with a membrane filter 301 for separating the catalyst in the liquid phase material, a product outlet 3010 is arranged on the side wall of the membrane filter 301 for discharging the purified product, the purified product coming out from the product outlet 3010 enters a first rectifying tower 4 for rectification to separate the product from the methanol, a tower top condenser 401 is arranged at the tower top of the first rectifying tower 4, a part of condensate coming out from the tower top condenser 401 returns to the first rectifying tower 4, a part of condensate is premixed to a tank 1, a heavy component outlet 42 is arranged at the tower bottom of the first rectifying tower 4, the product after the methanol is separated enters an extraction tower 50 from the heavy component outlet 42 for product extraction, an extraction solvent spray nozzle 501 is arranged at the top of the extraction tower 5, the organic solvent enters from the top of the extraction tower 5 and is extracted by spraying, the bottom of the extraction tower 50 is provided with an extraction liquid outlet 51, the extraction liquid enters into the second rectifying tower 6 after coming out from the extraction liquid outlet 51 to remove the extraction solvent, and the final product methyl myristate after removing the organic solvent is extracted from the bottom of the second rectifying tower 6.
In addition, the bottom of the complete mixing kettle 2 is provided with a first catalyst outlet 24, the bottom of the catalyst separator 3 is provided with a second catalyst outlet 32, and the outlets of the first catalyst outlet 24 and the second catalyst outlet 32 are communicated and recovered together, in this embodiment, the system further comprises a catalyst regenerator 7, and the side wall of the catalyst regenerator 7 is connected with the first catalyst outlet 24 and the second catalyst outlet 32 respectively; the side wall of the catalyst regenerator 7 is connected with the catalyst inlet 22 for the regenerated catalyst to return to the full mixing kettle 2 for utilization.
Example 2
The procedure of this example is identical to that of example 1, except that Amberlyst 39wet, a catalyst of 15% by weight of the mass of the mixture, is used.
Example 3
The procedure of this example is identical to that of example 1, except that 20% by weight of the mixture mass of catalyst Amberlyst 39wet is added. The gas chromatogram of the specific product is shown in FIG. 3.
Example 4
The procedure of this example was identical to that of example 1, except that Amberlyst 39wet, a catalyst amount of 25 wt% of the mixture mass, was used.
Example 5
The procedure of this example was identical to that of example 1, except that 30% by weight of the mixture mass of the catalyst Amberlyst 39wet was added.
As can be seen from FIG. 2, the contents of the solid acid catalysts of the present invention in the specific conditions of the amount of the mixture of 10-30 wt% in examples 1-5 are compared, so that the conversion rate of the product reaches 97.8% -99.7%, especially in the case of the amount of the mixture of 30 wt%, the conversion rate of the product reaches the highest 99.7%, and the optimal amount of the catalyst is 30 wt%.
Example 6
The procedure of this example is identical to that of example 1, except that Amberlyst 15wet, a catalyst in an amount of 10% by weight of the mixture mass, is added to the complete mixing tank 2.
Example 7
The procedure of this example is identical to that of example 1, except that Amberlyst 35wet, a catalyst amount of 10% by weight of the mixture mass, is added to the complete mixing tank 2.
Example 8
The procedure of this example is identical to that of example 1, except that Amberlyst 36wet, a catalyst in an amount of 10% by weight of the mixture mass, is added to the complete mixing tank 2.
Example 9
The procedure of this example is identical to that of example 1, except that Lewatit K2620 catalyst, 10% by weight of the mixture mass, is added to the full-mixing tank 2.
As is clear from FIG. 3, by changing the kind of catalyst, the solid acid catalyst Amberlyst 39wet showed the best activity and the highest yield of methyl myristate, compared with examples 6 to 9 and 1.
Example 10
The procedure of this example is identical to that of example 3, except that tetradecanoic acid and methanol are introduced into premix tank 1 at a molar ratio of 1:3, and the gas chromatogram of the specific product is shown in FIG. 4.
As can be seen from the gas chromatograms in FIGS. 4 and 5, the yield of methyl myristate obtained by using the scheme of the present invention is ideal.
In a word, the preparation method of the utility model uses the solid acid catalyst to replace the liquid acid catalyst, the specific surface area and the pore volume of the solid acid catalyst are both larger, good selectivity and reaction activity are ensured, the product is easy to separate and purify, the solid acid catalyst can be repeatedly used for many times, the corrosion of equipment and the environmental pollution are avoided, and the continuous production of enterprises is realized; under the specific condition of the catalyst dosage of 10-30 wt% of the mixture, the reaction efficiency is greatly improved, the occurrence of side reaction is inhibited, the conversion rate of the product can reach 97.8% -99.7%, and the yield and the quality of the final product methyl myristate are improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention.
Claims (4)
1. The system for preparing the methyl myristate is characterized by comprising a premixing tank for premixing raw materials, wherein the premixing tank is connected with a full mixing kettle, the full mixing kettle is provided with a catalyst inlet for introducing a solid acid catalyst and a raw material inlet for introducing the raw materials, and the full mixing kettle is provided with a temperature control device;
a product outlet is formed in the side wall of the full mixing kettle, and a reaction product enters a catalyst separator from the product outlet to separate and recover the catalyst;
the top of the catalyst separator is provided with a liquid phase outlet which is connected with a membrane filter for separating the catalyst in the liquid phase material;
the bottom of the membrane filter is provided with a catalyst recovery port, the side wall of the membrane filter is provided with a product outlet for discharging purified products, and the catalyst recovery port is connected with the side wall of the catalyst separator for returning part of materials to the catalyst separator for continuous purification and separation;
the bottom of the full mixing kettle is provided with a first catalyst outlet; a second catalyst outlet is formed in the bottom of the catalyst separator, and the second catalyst outlet is communicated with the first catalyst outlet for common recovery;
the system also comprises a catalyst regenerator, the side wall of the catalyst regenerator is respectively connected with the first catalyst outlet and the second catalyst outlet, and the side wall of the catalyst regenerator is connected with the catalyst inlet so that the regenerated catalyst returns to the full mixing kettle again.
2. The system of claim 1, wherein the product outlet is connected to a first rectification column for separating products from methanol; and a tower top condenser is arranged at the tower top of the first rectifying tower, part of condensate coming out of the tower top condenser returns to the first rectifying tower, and part of condensate goes to the premixing tank.
3. The system of claim 2, wherein a heavy component outlet is arranged at the bottom of the first rectifying tower, and an extraction tower is connected to the heavy component outlet for product extraction and purification.
4. The system of claim 3, wherein the top of the extraction tower is provided with an extraction solvent spray nozzle, the bottom of the extraction tower is provided with an extraction liquid outlet, and the extraction liquid outlet is connected with the second rectification tower for removing the extraction solvent.
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