阅读说明：本技术 一种肉豆蔻酸异丙酯的生产工艺 (Production process of isopropyl myristate ) 是由 马柏跃 徐跃邦 舒利贞 于 2020-12-31 设计创作，主要内容包括：本发明公开了一种肉豆蔻酸异丙酯的生产工艺,包括如下步骤：1、将肉豆蔻酸和异丙醇依次放入酯化反应釜中,加热搅拌；2、当反应釜中温度加热至45～55℃时向酯化反应釜中加入催化剂并继续加热搅拌,保持酯化反应釜内部温度在70～85℃,并持续反应4～6h,之后静置1～1.5h,并分离水分；3、静置后继续搅拌反应3～6h,得肉豆蔻酸异丙酯粗品；4、将步骤3中所得的肉豆蔻酸异丙酯粗品进行水洗、脱臭和脱色处理后进行成品包装即可；其中,所述酯化反应釜的内部设有水分分离机构,在步骤3中,待酯化反应釜内物料静置分层后,通过所述水分分离机构用于将酯化反应釜内反应的水分分离。本发明生产方法简单,且酯化反应产率高,产品纯度高,有利于工业化的生产应用。(The invention discloses a production process of isopropyl myristate, which comprises the following steps: 1. sequentially putting myristic acid and isopropanol into an esterification reaction kettle, and heating and stirring; 2. adding a catalyst into the esterification reaction kettle when the temperature in the reaction kettle is heated to 45-55 ℃, continuously heating and stirring, keeping the internal temperature of the esterification reaction kettle at 70-85 ℃, continuously reacting for 4-6 h, standing for 1-1.5 h, and separating water; 3. standing and then continuously stirring for reacting for 3-6 h to obtain a crude product of isopropyl myristate; 4. washing, deodorizing and decoloring the isopropyl myristate crude product obtained in the step 3, and packaging a finished product; and in step 3, after the materials in the esterification reaction kettle are kept standing and layered, the moisture separation mechanism is used for separating the moisture of the reaction in the esterification reaction kettle. The production method is simple, high in esterification reaction yield and high in product purity, and is beneficial to industrial production and application.)

1. A production process of isopropyl myristate comprises the following steps:

step 1, sequentially putting myristic acid and isopropanol into an esterification reaction kettle (1), and heating and stirring;

step 2, when the temperature in the reaction kettle is heated to 45-55 ℃, adding a catalyst into the esterification reaction kettle (1), continuously heating and stirring, keeping the internal temperature of the esterification reaction kettle (1) at 70-85 ℃, continuously reacting for 4-6 h, standing for 1-1.5 h, and separating water;

step 3, continuously stirring and reacting for 3-6 hours after standing to obtain a crude product of isopropyl myristate;

step 4, putting the isopropyl myristate crude product obtained in the step 3 into a washing kettle for washing treatment;

step 5, putting the isopropyl myristate crude product subjected to the water washing treatment in the step 4 into a deodorization kettle for deodorization treatment;

step 6, placing the crude isopropyl myristate subjected to deodorization treatment in the step 5 into a decoloring kettle for decoloring treatment to obtain a finished isopropyl myristate product, and finally packaging the finished product;

and in step 3, after the materials in the esterification reaction kettle are stood for layering, the moisture separation mechanism is used for separating the moisture of the reaction in the esterification reaction kettle.

2. The process according to claim 1, wherein the isopropyl myristate is prepared by the following steps: the moisture separating mechanism comprises a positioning plate (2), a sealing element (3) and a first driving mechanism (4), wherein the positioning plate (2) is fixed at the position inside the esterification reaction kettle (1) and close to the bottom end of the esterification reaction kettle (1), a positioning groove (5) is arranged at the top end axle center position of the positioning plate (2), an annular groove (6) arranged along the circumferential direction of the positioning groove (5) is arranged at the bottom end of the positioning groove (5), a plurality of liquid leaking holes (7) are uniformly distributed at the bottom end of the annular groove (6), a plurality of layers of nanofiber water-oil separating films (8) are laid inside the annular groove (6), the sealing element (3) is hollow inside and is provided with an open structure at the bottom end, the sealing element (3) is screwed in the positioning groove (5), a plurality of strip-shaped holes (9) which are arranged along the circumferential direction of the sealing element (3) and are communicated with the inside of the sealing element (3) are, the top of sealing member (3) is equipped with spliced pole (10), the top of spliced pole (10) runs through in the top of esterification reaction cauldron (1), first actuating mechanism (4) are including being fixed in the first motor on esterification reaction cauldron (1) top, the output of first motor is connected with the top transmission of spliced pole (10).

3. The process according to claim 2, wherein the isopropyl myristate is prepared by the following steps: the nanofiber water-oil separation membrane (8) is a water-absorbing and oil-dredging type nanofiber water-oil separation membrane.

4. The process according to claim 2, wherein the isopropyl myristate is prepared by the following steps: the bottom of esterification reaction cauldron (1) is equipped with outlet (11), the lateral wall of esterification reaction cauldron (1) is equipped with and is equipped with the discharge gate (12) that communicate with locating plate (2) inside constant head tank (5) corresponding to the position department of locating plate (2).

5. The process according to claim 2, wherein the isopropyl myristate is prepared by the following steps: esterification reaction cauldron (1) inside still is equipped with rabbling mechanism, the rabbling mechanism is located spliced pole (10) outside rotation sleeve (13), is fixed in and rotates stirring rake (14) of sleeve (13) outside and is fixed in second actuating mechanism (15) on esterification reaction cauldron (1) outside top including rotating the cover, the top of rotating sleeve (13) runs through in the top of esterification reaction cauldron (1) and is connected through belt transmission with second actuating mechanism (15).

6. The process according to claim 1, wherein the isopropyl myristate is prepared by the following steps: the catalyst is any one of concentrated sulfuric acid or p-methanesulfonic acid.

Technical Field

The invention relates to a production process of isopropyl myristate.

Background

Isopropyl myristate is an important long-chain carboxylic ester compound, has the excellent characteristics of low viscosity, no stimulation to skin, good intersolubility and the like, and is widely applied to the aspects of cosmetics, spices, insecticides, medicines, textiles and the like.

In the prior art, generally, myristic acid and isopropanol are used as raw materials in the production of isopropyl myristate, and esterification reaction is carried out under the action of a catalyst to form isopropyl myristate. Meanwhile, because the esterification reaction is not reversible, in the reaction process, in order to improve the yield of the product, a certain amount of water-carrying agent is generally added in the reaction to reduce the water content in the reaction product, so that the reaction is further driven to the direction of the esterification reaction to improve the yield of the product. However, after the water-carrying agent is added, unnecessary impurities are added in the product, so that the purity of the product is affected, and the requirements of people cannot be met.

Disclosure of Invention

The invention aims to solve the problems and provides a production process of isopropyl myristate, which is simple in production method, high in esterification reaction yield and high in product purity, and is beneficial to industrial production and application.

The invention adopts the following technical scheme:

a production process of isopropyl myristate comprises the following steps:

step 1, sequentially putting myristic acid and isopropanol into an esterification reaction kettle, and heating and stirring;

step 2, when the temperature in the reaction kettle is heated to 45-55 ℃, adding a catalyst into the esterification reaction kettle, continuously heating and stirring, keeping the internal temperature of the esterification reaction kettle at 70-85 ℃, continuously reacting for 4-6 h, standing for 1-1.5 h, and separating water;

step 3, continuously stirring and reacting for 3-6 hours after standing to obtain a crude product of isopropyl myristate;

step 4, putting the isopropyl myristate crude product obtained in the step 3 into a washing kettle for washing treatment;

step 5, putting the isopropyl myristate crude product subjected to the water washing treatment in the step 4 into a deodorization kettle for deodorization treatment;

step 6, placing the crude isopropyl myristate subjected to deodorization treatment in the step 5 into a decoloring kettle for decoloring treatment to obtain a finished isopropyl myristate product, and finally packaging the finished product;

and in step 3, after the materials in the esterification reaction kettle are stood for layering, the moisture separation mechanism is used for separating the moisture of the reaction in the esterification reaction kettle.

As a preferred technical scheme of the invention, the moisture separation mechanism comprises a positioning plate, a sealing element and a first driving mechanism, the positioning plate is fixed in the esterification reaction kettle and is close to the bottom end of the esterification reaction kettle, a positioning groove is arranged at the axis position of the top end of the positioning plate, an annular groove arranged along the circumferential direction of the positioning groove is arranged at the bottom of the positioning groove, a plurality of liquid leakage holes are uniformly distributed at the bottom end of the annular groove, a plurality of layers of nanofiber water-oil separation membranes are paved in the annular groove, the sealing element is hollow in the inner part and has an open bottom end, the sealing element is screwed in the positioning groove in a threaded manner, a plurality of strip-shaped holes arranged along the circumferential direction of the sealing element and communicated with the inner part of the sealing element are arranged on the side wall of the sealing element, a connecting column is arranged at the top end, the first driving mechanism comprises a first motor fixed at the top end of the esterification reaction kettle, and the output end of the first motor is in transmission connection with the top end of the connecting column.

As a preferable technical scheme of the invention, the nanofiber water-oil separation membrane is a water-absorbing and oleophobic nanofiber water-oil separation membrane.

As a preferred technical scheme of the invention, a water outlet is arranged at the bottom end of the esterification reaction kettle, and a discharge hole communicated with a positioning groove in the positioning plate is arranged on the side wall of the esterification reaction kettle and at a position corresponding to the positioning plate.

As a preferred technical scheme of the invention, a stirring mechanism is further arranged in the esterification reaction kettle, the stirring mechanism comprises a rotating sleeve rotatably sleeved outside the connecting column, a stirring paddle fixed outside the rotating sleeve and a second driving mechanism fixed at the top end outside the esterification reaction kettle, and the top end of the rotating sleeve penetrates through the top end of the esterification reaction kettle and is in transmission connection with the second driving mechanism through a belt.

In a preferred embodiment of the present invention, the catalyst is any one of concentrated sulfuric acid and p-methanesulfonic acid.

The invention has the beneficial effects that:

the production process method is simple, the production cost is low, and the obtained product has high yield and high purity; the water separation mechanism arranged in the esterification reaction kettle can effectively remove water generated by reaction during production, promote the reaction to further tend to the direction of esterification reaction so as to improve the yield of products, and simultaneously can avoid the situation that the water-carrying agent is added in reactants to add unnecessary impurities into the products, thereby improving the purity of the products.

Drawings

FIG. 1 is a schematic structural view of an esterification reaction kettle according to the present invention;

the symbols in the drawings illustrate that:

esterification reaction kettle 1, locating plate 2, sealing member 3, first actuating mechanism 4, constant head tank 5, annular 6, weeping hole 7, nanofiber water oil separating membrane 8, bar hole 9, spliced pole 10, outlet 11, discharge gate 12, rotating sleeve 13, stirring rake 14, second actuating mechanism 15.

Detailed Description

The invention will now be described in further detail with reference to the drawings and examples.

A production process of isopropyl myristate comprises the following steps:

step 1, sequentially putting myristic acid and isopropanol into an esterification reaction kettle 1, and heating and stirring;

step 2, when the temperature in the reaction kettle is heated to 45-55 ℃, adding a catalyst into the esterification reaction kettle, continuously heating and stirring, keeping the internal temperature of the esterification reaction kettle at 70-85 ℃ (in the actual production process, a person skilled in the art can determine the specific esterification reaction temperature within the temperature range according to actual needs), continuously reacting for 4-6 h (in the actual production process, a person skilled in the art can determine the specific esterification reaction time within the reaction time range according to actual needs), standing for 1-1.5 h to layer the moisture generated by the reaction and other materials, and then separating the moisture;

step 3, continuously stirring and reacting for 3-6 hours after standing to obtain a crude product of isopropyl myristate;

step 4, putting the isopropyl myristate crude product obtained in the step 3 into a washing kettle for washing treatment;

step 5, putting the isopropyl myristate crude product subjected to the water washing treatment in the step 4 into a deodorization kettle for deodorization treatment;

step 6, placing the crude isopropyl myristate subjected to deodorization treatment in the step 5 into a decoloring kettle for decoloring treatment to obtain a finished isopropyl myristate product, and finally packaging the finished product;

and in step 3, after the materials in the esterification reaction kettle are stood for layering, the moisture separation mechanism is used for separating the moisture of the reaction in the esterification reaction kettle.

More specifically, in this embodiment, the moisture separation mechanism includes a positioning plate 2, a sealing member 3 and a first driving mechanism 4, the positioning plate 2 is fixed inside the esterification reaction kettle 1 and is close to the bottom end of the esterification reaction kettle 1, specifically, in this embodiment, the positioning plate 2 and the esterification reaction kettle 1 are an integrally formed structure; a positioning groove 5 is arranged at the axis position of the top end of the positioning plate 2, an annular groove 6 is arranged at the bottom of the positioning groove 5 along the circumferential direction of the positioning groove 5, a plurality of liquid leakage holes 7 are uniformly distributed at the bottom end of the annular groove 6, and a plurality of layers of nanofiber water-oil separation membranes 8 are laid inside the annular groove 6;

sealing member 3 is equipped with the open-ended structure for inside cavity and bottom, 3 screw threads of sealing member connect in constant head tank 5 soon, just be equipped with between sealing member 3 and the constant head tank 5 and be used for improving the sealed pad of the sealed effect of junction between sealing member 3 and the constant head tank 5, be equipped with on the lateral wall of sealing member 3 a plurality of along the circumferential direction setting of sealing member 3 and with the inside communicating bar hole 9 of sealing member 3, the top of sealing member 3 is equipped with spliced pole 10, the top of spliced pole 10 runs through in esterification reaction cauldron 1's top, first actuating mechanism 4 is including being fixed in the first motor on esterification reaction cauldron top, the output of first motor is connected with the top transmission of spliced pole 10, and is further, first motor is lead screw step motor.

More specifically, a water outlet 11 is arranged at the bottom end of the esterification reaction kettle 1, and a discharge hole 12 communicated with the positioning groove 5 in the positioning plate 2 is arranged on the side wall of the esterification reaction kettle 1 and at a position corresponding to the positioning plate;

further specifically, 1 inside rabbling mechanism that still is equipped with of reation kettle, rabbling mechanism locates the outside rotation sleeve 13 of spliced pole 10, is fixed in the outside stirring rake 14 of rotation sleeve 13 and is fixed in the second actuating mechanism 15 on 1 outside top of reation kettle including rotating the cover, the top of rotating sleeve 14 runs through on the top of reation kettle 1 and is connected through belt transmission with second actuating mechanism 15, during the use, thereby second actuating mechanism 15 is used for driving and rotates sleeve 13 and set up stirring rake 14 on rotating sleeve 13 and rotate and stir 1 inside material of reation kettle.

More specifically, the catalyst is concentrated sulfuric acid or p-methanesulfonic acid, and in the actual application process, a person skilled in the art can determine the type of the catalyst according to actual needs.

The use process of the moisture separation mechanism is briefly described as follows:

in step 3, treat that the layering back is stood to the interior material of esterification reaction cauldron 1, drive spliced pole 10 and sealing member 3 through first motor and rotate and make sealing member 3 rebound, bar hole 9 exposes this moment, 1 bottom material of esterification reaction cauldron (moisture promptly) gets into in the constant head tank 5 through bar hole 9 in to get into between locating plate 2 and the 1 bottom of esterification reaction cauldron through weeping hole 7 under the effect of nanofiber water oil separating membrane 8, thereby reach the purpose with moisture separation. And (3) discharging the separated water after the reaction from the water outlet 11, and discharging the rest materials from the discharge hole 12.

The moisture separation mechanism is used for separating moisture of the reaction in the esterification reaction kettle.

Finally, it should be noted that: these embodiments are merely illustrative of the present invention and do not limit the scope of the present invention. In addition, other variations and modifications will be apparent to persons skilled in the art based on the foregoing description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.