阅读说明：本技术 一种用于固体二元酸单酯化的连续生产装置及其使用方法 (Continuous production device for mono-esterification of solid dibasic acid and use method thereof ) 是由 陈志明 李剑 杨效军 仲军实 钱继兵 杨如惠 赵东一 夏佳佳 孔祥林 王瑞琦 孙 于 2020-05-29 设计创作，主要内容包括：本发明公开了一种用于固体二元酸单酯化的连续生产装置及其使用方法,该装置包括称重料斗,称重料斗上依次连接有转阀、中间料斗、旋转给料器、液固配料罐、乳化设备、浆料缓冲罐、单酯化反应罐；该装置使用方法包括以下步骤：(S1)将甲醇溶液通入液固配料罐；(S2)将二元酸原料经由中间料斗、旋转给料器通入液固配料罐,将甲醇和二元酸原料在液固配料罐中混合后通入乳化设备,乳化后进入浆料缓冲罐；(S3)启动浆料缓冲罐向单酯化反应罐输送浆料,启动单酯化反应罐、循环加热器及回流喷射系统进行单酯化反应；(S4)调整单酯化反应罐的温度压力,取样分析物料合格后输送至后续单元。该装置实现了常温、常压下的连续化操作,提高了生产效率。(The invention discloses a continuous production device for mono-esterification of solid dibasic acid and a using method thereof, wherein the device comprises a weighing hopper, wherein the weighing hopper is sequentially connected with a rotary valve, an intermediate hopper, a rotary feeder, a liquid-solid batching tank, an emulsifying device, a slurry buffer tank and a mono-esterification reaction tank; the using method of the device comprises the following steps: (S1) introducing the methanol solution into a liquid-solid dosing tank; (S2) introducing the dibasic acid raw material into a liquid-solid mixing tank through an intermediate hopper and a rotary feeder, mixing the methanol and the dibasic acid raw material in the liquid-solid mixing tank, introducing the mixture into emulsifying equipment, and emulsifying the mixture and then introducing the mixture into a slurry buffer tank; (S3) starting a slurry buffer tank to convey slurry to a single esterification reaction tank, and starting the single esterification reaction tank, a circulating heater and a reflux injection system to perform single esterification reaction; (S4) adjusting the temperature and pressure of the mono-esterification reaction tank, sampling and analyzing the qualified materials, and conveying the qualified materials to a subsequent unit. The device realizes continuous operation at normal temperature and normal pressure, and improves the production efficiency.)

1. A continuous production device for mono-esterification of solid dibasic acid is characterized by comprising a weighing hopper (1), the weighing hopper (1) is sequentially connected with a rotary valve (3), an intermediate hopper (4), a rotary feeder (5), a liquid-solid material mixing tank (8), an emulsifying device (9), a slurry buffer tank (10) and a single esterification reaction tank (12), the liquid-solid dosing tank (8) receives the dibasic acid raw material transmitted by the rotary feeder (5) and the methanol solution transmitted by the methanol feeding pipe (7), the slurry buffer tank (10) is sent to a mono-esterification reaction tank (12) through a bottom material conveying pump (11), the mono-esterification reaction tank (12) is provided with a circulating heater (14) and a reflux injection system (13), the rotary valve (3) is arranged on a pipeline connected with the heavy hopper (1) and the middle hopper (4).

2. Continuous production plant for the monoesterification of solid dibasic acids according to claim 1, wherein said backflow injection system (13) is a monoesterification pump.

3. The continuous production apparatus for the mono-esterification of solid dibasic acid according to claim 1, wherein the mono-esterification reaction tank (12) has a reaction temperature of 120 ℃ and 160 ℃ and a reaction pressure of 0.6 to 1.7 MPa.

4. The continuous production device for the mono-esterification of solid dibasic acid according to claim 1, wherein the methanol feeding pipe (7) is provided with a methanol feeding flow control meter which is matched with the rotary valve (3) to control the feeding proportion of the used amount of the raw materials of the methanol and the dibasic acid.

5. The continuous production device for the mono-esterification of the solid dibasic acid according to claim 1 or 4, wherein the molar ratio of the raw materials of the methanol and the dibasic acid is 3-10: 1.

6. The continuous production unit for the mono-esterification of solid dibasic acids according to claim 1, wherein a first gate valve (2) is provided on the pipeline between the weighing hopper (1) and the rotary valve (3), and a second gate valve (6) is provided on the pipeline between the rotary feeder (5) and the liquid-solid dosing tank (8).

7. The continuous production device for the monoesterification of solid dibasic acids according to claim 1, wherein said emulsifying apparatus (9) is an emulsifying pump or an emulsifying machine, and a moving gear and a static gear rotating at high speed are provided in said emulsifying apparatus (9).

8. The continuous production apparatus for mono-esterification of solid dibasic acid according to claim 1, wherein the bottom of the slurry buffer tank (10) is provided with a reflux pump, and the use temperature is 15-55 ℃ and the pressure is 0.001-100 Kpag.

9. Use of a continuous production unit for the mono-esterification of solid dibasic acids according to claim 1, characterized in that it comprises the following steps:

(S1) introducing the methanol solution into a liquid-solid dosing tank (8) by using a methanol feeding pipe (7);

(S2) introducing the dibasic acid raw material into a liquid-solid mixing tank (8) through an intermediate hopper (4) and a rotary feeder (5), mixing the methanol and the dibasic acid raw material in the liquid-solid mixing tank (8), introducing the mixture into an emulsifying device (9), emulsifying by the emulsifying device (9), and introducing the mixture into a slurry buffer tank (10);

(S3) starting a slurry buffer tank (10) to convey slurry to a mono-esterification reaction tank (12), and starting the mono-esterification reaction tank (12), a circulating heater (14) and a reflux injection system to perform mono-esterification reaction;

(S4) adjusting the temperature and pressure of the mono-esterification reaction tank (12), sampling and analyzing the materials in the mono-esterification reaction tank, and conveying the qualified materials to a subsequent unit.

10. Use of the continuous production unit for the mono-esterification of solid dibasic acids according to claim 9, wherein the pressure of the start-up slurry buffer tank (10) in the steps S2, S3 is adjusted by both nitrogen and vent off-gas.

Technical Field

The invention relates to a production device for solid dibasic acid mono-esterification and a using method thereof, in particular to a continuous production device for solid dibasic acid mono-esterification and a using method thereof.

Background

1, 4-Butanediol (BDO) and 1, 6-Hexanediol (HDO) are important chemical raw materials and are one of important raw materials for various organic syntheses, dibasic acid and methanol are subjected to esterification hydrogenation, the first step of the process is a mono-esterification reaction of the dibasic acid and the methanol, succinic acid and adipic acid are solid powder at normal temperature and normal pressure, the succinic acid or the adipic acid and the methanol are slightly soluble at the normal temperature, and the molar ratio of acid to alcohol is 1: when the methanol and the succinic acid or the adipic acid are mixed according to the proportion of 3-4, the liquid-phase methanol and the succinic acid or the adipic acid solid in the mixed solution are not mutually soaked, the succinic acid or the adipic acid crystals settle at the bottom within dozens of seconds after the mixing and stirring are stopped, the methanol is clearly layered at the top, and uniform solution or slurry cannot be formed, so that the continuous conveying of the two is very difficult. The existing succinic acid or adipic acid feeding and dissolving method is an intermittent method, namely, a certain amount of methanol is firstly added into a pre-esterification reaction kettle, then succinic acid or adipic acid is added in proportion, after the succinic acid or adipic acid is heated, dissolved and reacted for 1-4 hours, the reaction liquid is sent into a pre-esterification buffer tank after the succinic acid or adipic acid is analyzed to be qualified and free of solid crystals, after the feeding is finished, a discharge valve is closed, an emptying valve is opened, after the pressure is reduced to normal pressure, the valve is opened, the next kettle solution preparation is carried out again, the pre-esterification reaction kettle cannot carry out continuous production, and the production efficiency is low; and the switching operation of two or more pre-esterification reaction kettles needs to be carried out, low-pressure steam is needed to be introduced for heating, and pressurization is needed to prevent methanol steam from reversely crossing to influence the feeding of the solid acid, so that the energy consumption is high.

Disclosure of Invention

The purpose of the invention is as follows: the invention aims to provide a continuous production device for mono-esterification of solid dibasic acid, which can realize continuous esterification operation, has high production efficiency and low energy consumption, and also aims to provide a using method of the device.

The technical scheme is as follows: the invention relates to a continuous production device for mono-esterification of solid dibasic acid, which comprises a weighing hopper, wherein a rotary valve, an intermediate hopper, a rotary feeder, a liquid-solid batching tank, emulsifying equipment, a slurry buffer tank and a mono-esterification reaction tank are sequentially connected onto the weighing hopper, the liquid-solid batching tank receives dibasic acid raw materials transmitted by the rotary feeder and methanol solution transmitted by a methanol feeding pipe, the slurry buffer tank is sent to the mono-esterification reaction tank through a bottom material conveying pump, a circulating heater and a reflux injection system are arranged on the mono-esterification reaction tank, and the rotary valve is arranged on a pipeline connected with the heavy hopper and the intermediate hopper.

Wherein, the reflux injection system is a mono-esterification pump, the reaction temperature of the mono-esterification reaction tank is 120-160 ℃, the reaction pressure is 0.6-1.7Mpa, and a methanol feed flow controller which is matched with a rotary valve to control the delivery proportion of the consumption of the methanol and the dibasic acid raw materials is arranged on the methanol feed pipe; the mol ratio of the methanol to the dibasic acid is 3-10: 1, a first gate valve is arranged on a pipeline between a weighing hopper and a rotary valve, a second gate valve is arranged on a pipeline between a rotary feeder and a liquid-solid mixing tank, the emulsifying equipment is an emulsifying pump or an emulsifying machine, a high-speed rotating dynamic and static gear is arranged in the emulsifying equipment, a reflux pump is arranged at the bottom of a slurry buffer tank, the use temperature is 15-55 ℃, and the pressure is 0.001-100 Kpag.

The use method of the continuous production device for the mono-esterification of the solid dibasic acid comprises the following steps:

(S1) introducing the methanol solution into a liquid-solid dosing tank by using a methanol feeding pipe;

(S2) introducing the dibasic acid raw material into a liquid-solid mixing tank through an intermediate hopper and a rotary feeder, mixing the methanol and the dibasic acid raw material in the liquid-solid mixing tank, introducing the mixture into emulsifying equipment, emulsifying by the emulsifying equipment, and introducing the mixture into a slurry buffer tank;

(S3) starting a slurry buffer tank to convey slurry to a single esterification reaction tank, and starting the single esterification reaction tank, a circulating heater and a reflux injection system to perform single esterification reaction;

(S4) adjusting the temperature and pressure of the mono-esterification reaction tank, sampling and analyzing the materials in the mono-esterification reaction tank, and conveying the qualified materials to a subsequent unit.

Wherein, the pressure of the starting slurry buffer tank in the steps S2 and S3 is adjusted by the nitrogen and the emptying tail gas together.

Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: 1. the batching and discharging processes are continuous, raw materials are emulsified into slurry under the working condition of high-speed cutting through emulsification equipment, and the slurry is continuously conveyed to a single esterification tank through a centrifugal pump, so that the continuous operation at normal temperature and normal pressure is realized, the problem of raw material deposition is avoided, and the production efficiency is improved; 2. the solid dibasic acid is cut into smaller crystals by emulsification equipment, so that the contact area with methanol is increased, and the reaction rate is improved; 3. the feeding ratio is controlled by using the rotary valve and a methanol feeding flow control meter, so that the problem that the rotary valve is blocked by solid dibasic acid due to methanol steam rising is avoided.

Drawings

FIG. 1 is a schematic diagram of the structure of the device of the present invention.

Detailed Description

Example 1

As shown in figure 1, the continuous production device for the mono-esterification of the solid dibasic acid comprises a weighing hopper 1, a rotary valve 3, an intermediate hopper 4, a rotary feeder 5, a liquid-solid batching tank 8, an emulsifying device 9, a slurry buffer tank 10 and a mono-esterification reaction tank 12, wherein the weighing hopper 1 and the rotary valve 3 are introduced into the intermediate hopper 4 through a dibasic acid feeding pipe, the rotary feeder 5 is communicated with a discharge hole of the intermediate hopper 4, the liquid-solid batching tank 8 receives a dibasic acid raw material transmitted by the rotary feeder 5 and a methanol solution transmitted by a methanol feeding pipe 7, the discharge of the liquid-solid batching tank 8 enters the emulsifying device 9, the discharge of the emulsifying device 9 enters the slurry buffer tank 10, the slurry buffer tank 10 is sent to the mono-esterification reaction tank 12 through a bottom material delivery pump 11, a circulating heater 14 and a backflow injection system 13 are arranged on the mono-esterification reaction tank 12, the rotary valve 3 is arranged on a pipeline connecting the weighing hopper 1 and the intermediate hopper 4, the backflow injection system 13 is a single esterification pump, a methanol feeding flow control meter is arranged on the methanol feeding pipe 7, the methanol feeding flow control meter and the rotary valve 3 are used for carrying out conveying proportion control on the using amount of methanol and dibasic acid raw materials, a first gate valve 2 is arranged on a pipeline between the weighing hopper 1 and the rotary valve 3, a second gate valve 6 is arranged on a pipeline between the rotary feeder 5 and the liquid-solid mixing tank 8, the emulsifying equipment 9 is an emulsifying pump with high-speed rotating dynamic and static gears inside, and a backflow pump is arranged at the bottom of the slurry buffer tank 10.

When in use, the feeding temperature of methanol is 40 ℃, a trace amount of nitrogen is filled to ensure that the operation is carried out under the micro positive pressure, the methanol enters a solid-liquid batching tank 8 through a methanol feeding pipe flow control meter through a methanol feeding pipe 7, is stirred by a stirrer and enters an emulsifying device 9, enters a slurry buffer tank 10 through an outlet of the emulsifying device 9, establishes a liquid level of 20 percent, starts a reflux pump of the slurry buffer tank 10 to circulate back to the slurry buffer tank 10, utilizes a bottom material conveying pump 11 to convey the methanol to a single esterification reaction tank 12 to establish a liquid level of 10 percent, starts a single esterification pump 13 at the bottom of the single esterification tank 12 to return to the single esterification reaction tank 12 through a circulating heater 14, leads adipic acid solid to enter an intermediate hopper 4 through a weighing hopper 1 and a first gate valve 2, before entering the intermediate hopper 4, controls the ratio of the methanol feeding flow control meter to a rotary valve 3 to control the molar ratio of the methanol to the adipic acid to be 3:1, and then enters the liquid-solid batching tank 8 through a rotary feeder 5 and a second gate valve 6, methanol and adipic acid are stirred, mixed and enter a feed inlet of an emulsifying device 9, the adipic acid is cut into smaller crystals through a high-speed rotating movable gear and a fixed gear inside the emulsifying device 9, the contact area with the methanol is increased, slurry formed by emulsifying the methanol and the adipic acid through the emulsifying device 9 enters a slurry buffer tank 10 through an outlet of the emulsifying device 9, the slurry buffer tank 10 continuously feeds the raw materials into a single esterification reaction tank 12 through a bottom material conveying pump 11 after the liquid level of the slurry buffer tank 10 reaches 50%, the pressure of the single esterification reaction tank 12 is set to be 0.85Mpag, the raw materials are heated through the single esterification pump and a circulating heater 14 and are conveyed back to the single esterification reaction tank 12, the temperature of the circulating heater 14 is set to be 130 ℃, the controller is automatically thrown, the single esterification reaction tank 12 reacts for 2 hours, and the materials are conveyed to a subsequent unit after being sampled and analyzed.

Example 2

This example differs from example 1 in that: the pressure in the mono-esterification reaction tank 12 was set at 1.08Mpag and the temperature controller for the cyclic heating was set at 140 ℃.

Example 3

This example differs from example 1 in that: the molar ratio of methanol to adipic acid was 4: 1.

Example 4

This example differs from example 3 in that: the pressure in the mono-esterification reaction tank 12 was set at 1.08Mpag and the temperature controller for the cyclic heating was set at 140 ℃.

Example 5

This example differs from example 1 in that: the molar ratio of methanol to adipic acid was 6:1, the pressure in the mono-esterification reaction tank 12 was set at 0.6pag, and the temperature controller for the cyclic heating was set at 120 ℃.

Example 6

This example differs from example 1 in that: the molar ratio of methanol to adipic acid was 10:1, the pressure in the mono-esterification reaction tank 12 was set at 1.7pag, and the temperature controller for the cyclic heating was set at 160 ℃.