CN104841348A - Continuous filter high pressure liquid and solid reaction device - Google Patents
Continuous filter high pressure liquid and solid reaction device Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 41
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- 239000007790 solid phase Substances 0.000 abstract description 5
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- 239000011949 solid catalyst Substances 0.000 description 7
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229920002367 Polyisobutene Polymers 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
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- 230000000717 retained effect Effects 0.000 description 2
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Abstract
本发明涉及了一种连续过滤式高压液固反应装置。本装置包括反应釜、至少两个过滤头、至少两个电动三通阀、液体进料管、液体出料管、压力传感器、阀门控制器和固体物料放料口；过滤头置于反应釜内壁上，每个过滤头与一个电动三通阀连接，液体进料管分别连接各个电动三通阀，液体出料管分别连接各个电动三通阀，压力传感器一端与反应釜连接，一端与阀门控制器连接，阀门控制器与电动三通阀连接，阀门控制器控制电动三通阀阀口的开和关，反应釜底部设置有固体物料放料口。本发明可以实现在较高操作压力下的连续反应，并且可方便地实现液固相的分离。装置简单，操作稳定，安全节能，可广泛地应用于多相催化、液固分离等化工生产过程中。
The invention relates to a continuous filtering high-pressure liquid-solid reaction device. The device includes a reaction kettle, at least two filter heads, at least two electric three-way valves, a liquid feed pipe, a liquid discharge pipe, a pressure sensor, a valve controller and a solid material discharge port; the filter head is placed on the inner wall of the reaction kettle Each filter head is connected to an electric three-way valve, the liquid feed pipe is connected to each electric three-way valve, the liquid discharge pipe is connected to each electric three-way valve, one end of the pressure sensor is connected to the reactor, and the other end is connected to the valve control The valve controller is connected with the electric three-way valve, the valve controller controls the opening and closing of the electric three-way valve port, and the bottom of the reactor is provided with a solid material discharge port. The invention can realize continuous reaction under higher operating pressure, and can conveniently realize the separation of liquid and solid phases. The device is simple, stable in operation, safe and energy-saving, and can be widely used in chemical production processes such as heterogeneous catalysis and liquid-solid separation.
Description
技术领域 technical field
本发明属于化工反应装置领域，特别涉及了一种连续过滤式高压液固反应装置。 The invention belongs to the field of chemical reaction devices, and in particular relates to a continuous filtering high-pressure liquid-solid reaction device.
背景技术 Background technique
反应釜主要应用于医药、燃料、农药、橡胶以及石油化工中的缩合、聚合、烃化、氢化、硝化以及磺化等工艺。液固相催化反应中，催化剂通常为固体，反应原料和产物为液态。对于特殊的工艺条件，如要求系统有较高的操作压力；反应过程连续，即连续进料，连续出料；反应结束后固体颗粒与液体物料分离。对于这样的操作条件，普通的反应釜难以满足要求。尤其对于颗粒细小的胶粘状固体，则液固相物料的分离比较困难，常用的过滤装置极易被堵塞。 Reactors are mainly used in condensation, polymerization, alkylation, hydrogenation, nitration and sulfonation processes in medicine, fuel, pesticide, rubber and petrochemical industry. In the liquid-solid phase catalytic reaction, the catalyst is usually solid, and the reaction raw materials and products are liquid. For special process conditions, if the system is required to have a higher operating pressure; the reaction process is continuous, that is, continuous feeding and continuous discharging; after the reaction, the solid particles are separated from the liquid materials. For such operating conditions, ordinary reactors are difficult to meet the requirements. Especially for sticky solids with fine particles, the separation of liquid and solid phase materials is difficult, and commonly used filter devices are easily blocked.
专利报道的一种全系统密闭高压连续式过滤工艺及装置（CN201115804Y）虽然可满足上述要求，但由于采用了高压气体反冲来解决滤网堵塞问题，增加了较多附属设备和装置，如往复泵、贮液罐、稳压罐、压力控制器、充气阀、脉冲控制器、电磁阀等。使整个系统显得十分复杂，不仅设备成本较高，也增加了很多操作费用。 A whole-system closed high-pressure continuous filtration process and device (CN201115804Y) reported in the patent can meet the above requirements, but due to the use of high-pressure gas recoil to solve the problem of filter blockage, more auxiliary equipment and devices have been added, such as reciprocating Pumps, liquid storage tanks, surge tanks, pressure controllers, charging valves, pulse controllers, solenoid valves, etc. Make the whole system seem very complicated, not only the equipment cost is higher, but also increased a lot of operating costs.
针对上述问题，本发明提供了一种连续过滤式高压液固反应装置，可以实现在较高操作压力下的连续反应，并且可方便地实现液固相的分离。装置简单，操作稳定，安全节能，可广泛地应用于多相催化、液固分离等化工生产过程中。 In view of the above problems, the present invention provides a continuous filter type high-pressure liquid-solid reaction device, which can realize continuous reaction under relatively high operating pressure, and can conveniently realize the separation of liquid and solid phases. The device is simple, stable in operation, safe and energy-saving, and can be widely used in chemical production processes such as heterogeneous catalysis and liquid-solid separation.
发明内容 Contents of the invention
本发明的目的是提供一种连续过滤式高压液固反应釜，实现液相和固相反应过程在高压密闭条件下的连续操作和反应，同时在生产过程中，方便连续地实现液固物料的分离。 The purpose of the present invention is to provide a continuous filter high-pressure liquid-solid reaction kettle, which can realize the continuous operation and reaction of the liquid phase and solid phase reaction process under high-pressure airtight conditions, and at the same time, in the production process, the liquid-solid material can be conveniently and continuously realized. separate.
为了实现上述目的本发明提供一种连续过滤式高压液固反应装置，包括反应釜、至少两个过滤头、至少两个电动三通阀、液体进料管、液体出料管、压力传感器、阀门控制器和固体物料放料口。过滤头置于反应釜内壁上，每个过滤头与一个电动三通阀连接，液体进料管分别连接各个电动三通阀，液体出料管分别连接各个电动三通阀，压力传感器一端与反应釜连接，一端与阀门控制器连接，阀门控制器与电动三通阀连接，阀门控制器控制电动三通阀阀口的开和关，反应釜底部设置有固体物料放料口。阀门控制器通过电动三通阀控制料液的进料和出料；电动三通阀上连接过滤头的阀口常开；若干电动三通阀上连接进料管的阀口打开，连接出料管的阀口关闭，同时其余的电动三通阀上连接进料管的阀口关闭，连接出料管的阀口打开；当反应釜内压力增大，压差信号通过压力传感器传递到阀门控制器，阀门控制器控制所述若干电动三通阀上连接进料管的阀口由打开切换为关闭，连接出料管的阀口由关闭切换为打开，同时所述其余的电动三通阀上连接进料管的阀口由关闭切换为打开，连接出料管的阀口由打开切换为关闭。过滤头为2个。 In order to achieve the above object, the present invention provides a continuous filtration high-pressure liquid-solid reaction device, including a reaction kettle, at least two filter heads, at least two electric three-way valves, a liquid feed pipe, a liquid discharge pipe, a pressure sensor, a valve Controller and solid material discharge port. The filter head is placed on the inner wall of the reactor, each filter head is connected to an electric three-way valve, the liquid feed pipe is respectively connected to each electric three-way valve, the liquid discharge pipe is respectively connected to each electric three-way valve, and one end of the pressure sensor is connected to the reaction valve. The kettle is connected, one end is connected to the valve controller, the valve controller is connected to the electric three-way valve, the valve controller controls the opening and closing of the electric three-way valve port, and the bottom of the reaction kettle is provided with a solid material discharge port. The valve controller controls the feed and discharge of the liquid through the electric three-way valve; the valve port connected to the filter head on the electric three-way valve is normally open; the valve port connected to the feed pipe on several electric three-way valves is opened, and the valve port connected to the discharge The valve port of the pipe is closed, while the valve port connected to the feed pipe on the other electric three-way valves is closed, and the valve port connected to the discharge pipe is opened; when the pressure in the reactor increases, the pressure difference signal is transmitted to the valve control through the pressure sensor The valve controller controls the valve ports connected to the feed pipes on the several electric three-way valves to switch from open to closed, and the valve ports connected to the discharge pipes to switch from closed to open, while the rest of the electric three-way valves The valve port connected to the feed pipe is switched from closed to open, and the valve port connected to the discharge pipe is switched from open to closed. There are 2 filter heads.
本发明的一个操作周期分为两个阶段。 An operation cycle of the present invention is divided into two stages.
固体物料放入反应釜后，封闭反应釜。 After the solid material is put into the reactor, close the reactor.
第一阶段：将料液通过液体进料管（3），第一电动三通阀（6-1），第一过滤头（2-1），送入反应釜（1）内，与固体物料进行接触反应。反应后的料液通过第二过滤头（2-2），第二电动三通阀（6-2），由液体出料管（4）放出。此时反应釜（1）内的固体物料被第二过滤头（2-2）拦截滞留于反应釜内。 The first stage: feed the liquid into the reaction kettle (1) through the liquid feed pipe (3), the first electric three-way valve (6-1), and the first filter head (2-1), and mix with the solid material Perform a contact reaction. The reacted feed liquid passes through the second filter head (2-2), the second electric three-way valve (6-2), and is released from the liquid discharge pipe (4). At this time, the solid material in the reactor (1) is intercepted and retained in the reactor by the second filter head (2-2).
第二阶段：经过一段时间的运行，固体物料会堵塞第二过滤头（2-2），使釜内压力增大，当增大到一定的压力时，压差信号通过压力传感器（7）传递到阀门控制器（5），阀门控制器（5）控制第一电动三通阀（6-1）和第二电动三通阀（6-2）同时切换方向，此时料液改从第二电动三通阀（6-2），第二过滤头（2-2），送入反应釜（1）内，反应后的液体通过第一过滤头（2-1），第一电动三通阀（6-1），由液体出料管（4）放出。由于液体流向的改变，料液从第二过滤头（2-2）进料，使在第一阶段操作过程中堵塞在第二过滤头（2-2）中的固体颗料被反洗下来，带入反应釜（1）中，第二过滤头（2-2）畅通。 The second stage: After a period of operation, the solid material will block the second filter head (2-2), which will increase the pressure in the kettle. When it reaches a certain pressure, the pressure difference signal will be transmitted through the pressure sensor (7) To the valve controller (5), the valve controller (5) controls the first electric three-way valve (6-1) and the second electric three-way valve (6-2) to switch directions at the same time, at this time the feed liquid changes from the second The electric three-way valve (6-2), the second filter head (2-2), is sent into the reactor (1), and the reacted liquid passes through the first filter head (2-1), and the first electric three-way valve (6-1), discharged from the liquid discharge pipe (4). Due to the change of the liquid flow direction, the feed liquid is fed from the second filter head (2-2), so that the solid particles blocked in the second filter head (2-2) are backwashed during the first stage operation, Bring it into the reaction kettle (1), and the second filter head (2-2) is unblocked.
再经过一段时间的运行，固体物料会堵塞第一过滤头（2-1），使釜内压力增大，压差信号通过压力传感器（7）传递到阀门控制器（5），阀门控制器（5）控制第一电动三通阀（6-1）和第二电动三通阀（6-2）同时切换方向，此时料液改从第一电动三通阀（6-1），第一过滤头（2-1），进入反应釜（1）内，反应后的液体通过第二过滤头（2-2），第二电动三通阀（6-2），由液体出料管（4）放出。此时料液从第一过滤头（2-1）进料，使得在第二阶段操作过程中堵塞在第一过滤头（2-1）中的固体颗料被反洗下来，带入反应釜（1）中，第一过滤头（2-1）畅通。 After a period of operation, the solid material will block the first filter head (2-1), which will increase the pressure in the kettle, and the pressure difference signal will be transmitted to the valve controller (5) through the pressure sensor (7), and the valve controller ( 5) Control the first electric three-way valve (6-1) and the second electric three-way valve (6-2) to switch directions at the same time. At this time, the feed liquid is changed from the first electric three-way valve (6-1) to the first The filter head (2-1) enters the reactor (1), and the reacted liquid passes through the second filter head (2-2), the second electric three-way valve (6-2), and is discharged from the liquid discharge pipe (4 )release. At this time, the feed liquid is fed from the first filter head (2-1), so that the solid particles blocked in the first filter head (2-1) during the second stage of operation are backwashed and brought into the reactor In (1), the first filter head (2-1) is unblocked.
上述过程反复进行，直至固体物料需排出，通过放料口（8）放出为止。 The above process is repeated until the solid material needs to be discharged through the discharge port (8).
本发明的特点是： The features of the present invention are:
（1）可以实现在高压密闭条件下的液固两相的连续反应； (1) It can realize the continuous reaction of liquid-solid two-phase under high pressure and airtight conditions;
（2）采用过滤头截留固体物料，实现液固两相的连续分离； (2) The filter head is used to intercept solid materials to realize the continuous separation of liquid and solid two phases;
（3）采用阀门控制器自动控制电动三通阀控制液体的进料和出料，使料液交替通过两个过滤头，实现进料的同时进行反冲洗，冲洗掉上一个阶段操作过程中堵塞在过滤头的固体物料，保持过滤头始终畅通； (3) The valve controller is used to automatically control the electric three-way valve to control the feeding and discharging of the liquid, so that the feeding liquid alternately passes through the two filter heads, so as to realize backwashing while feeding, and flush out the blockage in the previous stage of operation. For the solid material in the filter head, keep the filter head unblocked all the time;
（4）反应装置结构简单，无附属设备，造价低廉，可靠性高，易维护。 (4) The reaction device has a simple structure, no auxiliary equipment, low cost, high reliability and easy maintenance.
本发明的有益效果是：本发明提供了一种连续过滤式高压液固反应装置，可以实现在较高操作压力下的连续反应，并且可方便地实现液固相的分离。装置简单，操作稳定，安全节能，可广泛地应用于多相催化、液固分离等化工生产过程中。 The beneficial effects of the present invention are: the present invention provides a continuous filtering high-pressure liquid-solid reaction device, which can realize continuous reaction under relatively high operating pressure, and can conveniently realize the separation of liquid and solid phases. The device is simple, stable in operation, safe and energy-saving, and can be widely used in chemical production processes such as heterogeneous catalysis and liquid-solid separation.
附图说明 Description of drawings
图1是一种连续过滤式高压液固反应装置示意图。 Figure 1 is a schematic diagram of a continuous filtration high-pressure liquid-solid reaction device.
图中：1、反应釜；2-1、第一过滤头；2-2、第二过滤头；3、液体进料管；4、液体出料管；5、阀门控制器；6-1、第一电动三通阀；6-2、第二电动三通阀；7、压力传感器；8、固体物料放料口。 In the figure: 1. Reactor; 2-1. First filter head; 2-2. Second filter head; 3. Liquid feed pipe; 4. Liquid discharge pipe; 5. Valve controller; 6-1. The first electric three-way valve; 6-2, the second electric three-way valve; 7, the pressure sensor; 8, the solid material discharge port.
具体实施方式 Detailed ways
下面结合附图进一步说明本发明的实施过程。下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。 The implementation process of the present invention will be further described below in conjunction with the accompanying drawings. The following non-limiting examples can enable those skilled in the art to understand the present invention more fully, but do not limit the present invention in any way.
实施例1 Example 1
连续过滤式高压液固反应装置用于聚异丁烯催化反应，反应装置见附图1，包括反应釜（1），第一过滤头（2-1）、第二过滤头（2-2），液体进料管（3），液体出料管（4），阀门控制器（5），第一电动三通阀（6-1），第二电动三通阀（6-2），压力传感器（7）和固体物料放料口（8）。 The continuous filtration high-pressure liquid-solid reaction device is used for the catalytic reaction of polyisobutylene. The reaction device is shown in Figure 1, including the reaction kettle (1), the first filter head (2-1), the second filter head (2-2), the liquid Feed pipe (3), liquid discharge pipe (4), valve controller (5), first electric three-way valve (6-1), second electric three-way valve (6-2), pressure sensor (7 ) and solid material discharge port (8).
反应釜（1）为不锈钢，体积10 L。反应原料为混合液态烃（含异丁烯28.1%）和固载于γ－Al2O3上的AlCl3催化剂（以下简称固体催化剂）。 The reaction kettle (1) is stainless steel with a volume of 10 L. The raw materials for the reaction are mixed liquid hydrocarbons (containing 28.1% isobutene) and AlCl 3 catalysts (hereinafter referred to as solid catalysts) loaded on γ-Al 2 O 3 .
将固体催化剂0.4 kg放入反应釜（1）后，封闭反应釜（1）。将混合液态烃以10 L/h的流速通过液体进料管（3），第一电动三通阀（6-1 ），第一过滤头（2-1），送入反应釜（1）内，与固体催化剂进行接触反应。反应釜内温度20oC，压力10 MPa。反应后的料液通过第二过滤头（2-2），第二电动三通阀（ 6-2），由液体出料管（4）放出。此时反应釜（1）内的固体催化剂被第二过滤头（2-2）拦截滞留于反应釜内。 After putting 0.4 kg of solid catalyst into the reactor (1), close the reactor (1). Send the mixed liquid hydrocarbons through the liquid feed pipe (3), the first electric three-way valve (6-1), and the first filter head (2-1) at a flow rate of 10 L/h, and send them into the reaction kettle (1) , with a solid catalyst for contact reaction. The temperature in the reactor is 20 o C, and the pressure is 10 MPa. The reacted feed liquid passes through the second filter head (2-2), the second electric three-way valve (6-2), and is released from the liquid discharge pipe (4). At this time, the solid catalyst in the reactor (1) is intercepted and retained in the reactor by the second filter head (2-2).
经过一段时间的运行，固体物料会堵塞第二过滤头（2-2），使釜内压力增大，当增大到12Mpa时，压差信号通过压力传感器（7）传递到阀门控制器（5），阀门控制器（5）控制第一电动三通阀（6-1）和第二电动三通阀（6-2）同时切换方向，此时混合液态烃改从第二电动三通阀（6-2），第二过滤头（2-2），进入反应釜（1）内，反应后的液态烃通过第一过滤头（2-1），第一电动三通阀（ 6-1），由液体出料管（4）放出。由于进料流向的改变，液态烃从第二过滤头（2-2）进料，使在第一阶段操作过程中堵塞在第二过滤头（2-2）中的固体催化剂被反洗下来，带入反应釜（1）中，第二过滤头（2-2）畅通。 After a period of operation, the solid material will block the second filter head (2-2), which will increase the pressure in the kettle. When it increases to 12Mpa, the differential pressure signal will be transmitted to the valve controller (5) through the pressure sensor (7) ), the valve controller (5) controls the direction of the first electric three-way valve (6-1) and the second electric three-way valve (6-2) to switch simultaneously. 6-2), the second filter head (2-2), enters the reactor (1), the liquid hydrocarbons after the reaction pass through the first filter head (2-1), the first electric three-way valve (6-1) , released from the liquid discharge pipe (4). Due to the change of feed flow direction, liquid hydrocarbons are fed from the second filter head (2-2), so that the solid catalyst blocked in the second filter head (2-2) during the first stage operation is backwashed down, Bring it into the reaction kettle (1), and the second filter head (2-2) is unblocked.
当第一过滤头（2-1）出现堵塞时，釜内压力增大，当增大到12Mpa时，压差信号通过压力传感器（7）传递到阀门控制器（5），阀门控制器（5）控制第一电动三通阀（6-1）和第二电动三通阀（6-2）同时切换方向，此时液态烃改从第一电动三通阀（6-1），第一过滤头（2-1），进入反应釜（1）内，反应后的液态烃通过第二过滤头（2-2），第二电动三通阀（ 6-2），进入液体出料管（4）放出。此时液态烃由第一过滤头（2-1）进料，使在第二阶段操作过程中堵塞在第一过滤头（2-1）中的固体颗料被反洗下来，带入反应釜（1）中，第一过滤头（ 2-1）畅通。 When the first filter head (2-1) is clogged, the pressure in the kettle increases, and when it increases to 12Mpa, the differential pressure signal is transmitted to the valve controller (5) through the pressure sensor (7), and the valve controller (5 ) to control the first electric three-way valve (6-1) and the second electric three-way valve (6-2) to switch direction at the same time. Head (2-1), into the reactor (1), the liquid hydrocarbon after the reaction through the second filter head (2-2), the second electric three-way valve (6-2), into the liquid discharge pipe (4 )release. At this time, liquid hydrocarbons are fed from the first filter head (2-1), so that the solid particles blocked in the first filter head (2-1) during the second stage of operation are backwashed and brought into the reactor (1), the first filter head (2-1) is unblocked.
经过连续过滤式高压液固反应装置，混合液态烃（含异丁烯28.1%）和固载于γ－Al2O3上的AlCl3催化剂反应后生成聚异丁烯，测得转化率达89.1%，聚异丁烯分子量为870。 After a continuous filtration high-pressure liquid-solid reaction device, mixed liquid hydrocarbons (containing 28.1% isobutene) reacted with AlCl 3 catalyst solidly supported on γ-Al 2 O 3 to form polyisobutene, and the measured conversion rate reached 89.1%. Polyisobutene The molecular weight is 870.
上述过程反复进行，直至固体催化剂使用约1000 h，需排出进行再生为止。固体催化剂通过固体物料放料口（8）放出后进行再生处理。 The above process is repeated until the solid catalyst has been used for about 1000 hours and needs to be discharged for regeneration. The solid catalyst is discharged through the solid material discharge port (8) and then regenerated.
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