CN216837837U - Shell-and-tube crystallizer and continuous paraffin crystallization separation device - Google Patents
Shell-and-tube crystallizer and continuous paraffin crystallization separation device Download PDFInfo
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Abstract
A shell-and-tube crystallizer and a continuous paraffin crystallization separation device, the shell-and-tube crystallizer, divide the space in the body into lower product melting chamber (I) and upper liquid phase collecting chamber (II) by the baffle (100), the heat exchange tube (301) runs through the space in the body, set up the filter tube (302) in the said liquid phase collecting chamber, the top of the said filter tube is closed, the bottom opening communicates with product melting chamber, many heat exchange tubes and many filter tubes are staggered; the heat exchange medium inlet (105) and the heat exchange medium outlet (101) are respectively arranged at two ends of the shell and are communicated through the heat exchange tubes, the product melting chamber is provided with a raw material inlet (102) and a wax product outlet (104), and the lower part of the liquid phase collecting chamber is provided with a liquid phase outlet (103). The utility model provides a shell and tube crystallizer simple structure, easy and simple to handle, crystallization efficiency is high. The operation of a plurality of tubular crystallizers in parallel can realize continuous operation.
Description
Technical Field
The invention relates to equipment in the technical field of special wax production, in particular to a crystallizer for separating petroleum wax components.
Background
The phase-change energy storage material is a material capable of absorbing or emitting heat in a certain temperature range so as to achieve energy storage and release, and the phase-change wax is most widely applied. The phase-change wax is a special wax with a phase-change temperature of 20-80 ℃, is an excellent organic phase-change energy storage material, has the advantages of good heat storage performance, wide raw material source, low price and the like, is non-toxic and non-corrosive, and can be applied to the fields of building materials, solar energy, industrial waste heat utilization, temperature-adjusting textiles, the electronic industry, modern agriculture, medical care and the like. At present, the domestic phase-change wax industry has the problems that low-end products are excessive, the melting range is less than 10 ℃, and high-end products with phase-change enthalpy more than 200J/g are scarce.
The main component of the phase change wax is n-alkane (C)nH2n+2) The production raw material source mainly comprises two main types, one is petroleum wax, and the raw material is usually required to be subjected to solvent dewaxing to improve the normal hydrocarbon content of the raw material so as not to influence the enthalpy value of a product; another kind of commonly used raw material is Fischer-Tropsch wax, which is characterized by relatively simple composition, and normal straight-chain paraffin content up to 90% or more, basically noContains cyclic hydrocarbon and aromatic hydrocarbon, and is a high-quality phase-change wax production raw material.
The phase-change wax is produced mainly through purifying normal paraffin with corresponding carbon number from material, and the common purification includes distillation separation and crystallization separation. Distillation separation is a common mixture separation method, and the boiling range of the product can be reduced by the distillation method, so that the carbon number distribution range in the hydrocarbon product is effectively reduced, but the normal isomerization separation of the hydrocarbon species is not greatly influenced. CN 112745959a discloses a method for purifying paraffin by molecular distillation, which utilizes a method combining thin film evaporation and molecular distillation to purify paraffin. The crystallization separation is to separate the mixture by utilizing the difference of melting point properties of different components, such as normal isomerization separation of alkane, and normal alkane separation with different carbon numbers. The crystallization separation is widely applied to the production of phase-change wax, and particularly, a great deal of literature reports on the development aspect of crystallization equipment, CN 102977917A discloses a high-efficiency paraffin sweating device, CN 203284375A discloses a novel tubular paraffin deoiling device, CN 105754658A discloses a sweating crystallization method, the crystallization efficiency is improved by adopting water padding, solid particles are fully paved on the surface of a wax layer, and a forced airflow carries liquid components, and CN 109810725A also adopts a similar method. These are all improvements in the crystallization equipment and process. However, the phase-change wax product with high normal hydrocarbon content and narrow carbon number distribution can not be obtained by the crystallization method.
In order to obtain a wax product with a high normal hydrocarbon content and a narrow carbon number distribution, further optimization of the crystallization equipment used in the sweating separation process is required.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to provide a shell and tube crystallizer for producing high normal hydrocarbon content, narrow carbon number distribution.
The utility model provides a shell and tube crystallizer, by baffle 100 divide the space in the casing into lower part product melting chamber I and upper portion liquid phase collecting chamber II, heat exchange tube 301 link up the space in the casing, the liquid phase collecting chamber in set up filter tube 302, the filter tube top seal, the bottom opening communicates with each other with the product melting chamber, many heat exchange tubes and many filter tubes staggered arrangement; the heat exchange medium inlet 101 and the heat exchange medium outlet 105 are respectively arranged at two ends of the shell and are communicated through the heat exchange tubes, the product melting chamber is provided with a raw material inlet 102 and a product outlet 104, and the lower part of the liquid phase collecting chamber is provided with a liquid phase outlet 103.
The utility model provides a tubular crystallizer's application method does: firstly, a cooling medium is introduced through a heat exchange medium inlet 101, and the crystallizer is cooled through a heat exchange pipe 301 and then extracted through a pipeline 105. The material to be crystallized is introduced into the product melting chamber I from the raw material inlet 102, and the normal alkane therein is solidified and separated out due to cooling. After the product melting chamber I is filled with the liquid-solid mixed material, the liquid phase mainly containing isoparaffin at the upper layer enters the filter pipe 302, gradually enters the liquid phase collection chamber II through the filter pipe 302, is extracted through the liquid phase outlet 103 and is collected. And stopping feeding of the raw material inlet after the product melting chamber I is filled with the solid-phase product, introducing a heating medium through the heat exchange medium inlet 101 to heat the crystallizer, melting the solid-phase product in the product melting chamber I into a liquid phase, and collecting the liquid phase serving as the crystallized n-alkane product through the product outlet 104. Stopping extracting after all the liquid after melting is extracted, and finishing single batch operation.
A continuous paraffin crystallization and separation device is formed by connecting at least two shell-and-tube crystallizers in parallel.
The utility model provides a continuous paraffin crystallization separator's application method does:
two or more shell-and-tube crystallizers provided by the novel device are arranged in parallel, and are subjected to linkage control through liquid-solid interface/liquid level detection signals and material inlet and outlet valve switching. For example, two tubular crystallizers are arranged in parallel, when the first crystallizer is used for cooling crystallization, the other second crystallizer is used for melting discharge; after the second crystallizer finishes melting and discharging, introducing a cooling medium into the second crystallizer to be in a standby state; and after the first crystallizer is filled with the solid-phase material, the feeding is switched to the second crystallizer, and meanwhile, the first crystallizer is filled with the heating material to melt and extract the product, so that the continuous operation of raw material feeding and product extraction is realized.
The utility model provides a pair of shell-and-tube crystallizer and continuous paraffin crystallization separator's beneficial effect does:
the utility model provides a shell and tube crystallizer's simple structure has convenient operation, characteristics that crystallization efficiency is high. The utility model provides a continuous paraffin separation crystallization device can realize the operation of continuous feeding ejection of compact, guarantees the serialization operation of device.
Drawings
Fig. 1 is a schematic structural diagram of a shell-and-tube crystallizer provided by the present invention.
FIG. 2 is a schematic view of one arrangement of the filter tubes and heat exchange tubes in the product melting chamber.
Reference numerals:
i-a product melting chamber and II-a liquid phase collecting chamber.
100-partition plate, 101-heat exchange medium outlet, 102-raw material inlet, 103-liquid phase outlet, 104-product outlet, 105-heat exchange medium inlet, 106-upper end enclosure, 107-lower end enclosure, 108-fin, 301-heat exchange tube, 302-filter tube.
Detailed Description
The following describes the embodiments of the present invention in detail.
In the present application, the terms "upper", "lower" and "bottom" are used in reference to the relative positional relationship of the container or the member. Wherein, the upper part refers to the position of 50-100% of the container from bottom to top, and the lower part refers to the position of 0-50% of the container from bottom to top. The bottom refers to the position of 0-10% of the container from bottom to top, and the top refers to the position of 90-100% of the container from bottom to top.
In a first aspect, the present invention provides a shell-and-tube crystallizer, wherein a space inside a shell is divided into a lower product melting chamber i and an upper liquid phase collecting chamber ii by a partition plate 100, a heat exchange tube 301 penetrates through the space inside the shell, a filter tube 302 is disposed inside the liquid phase collecting chamber, the top of the filter tube is closed, the bottom opening of the filter tube is communicated with the product melting chamber, and a plurality of heat exchange tubes and a plurality of filter tubes are arranged in a staggered manner; the heat exchange medium inlet 105 and the heat exchange medium outlet 101 are respectively arranged at two ends of the shell and are communicated through the heat exchange tubes, the product melting chamber is provided with a raw material inlet 102 and a wax product outlet 104, and the lower part of the liquid phase collecting chamber is provided with a liquid phase outlet 103.
Preferably, the aperture of the filter pipe is 0.1-100 microns;
preferably, the filter tube is selected from a metal sintered tube or a ceramic membrane tube.
Preferably, the total cross-sectional area of the filter tubes accounts for 10-30% of the cross-sectional area of the liquid phase collection chamber, and the total cross-sectional area of the heat exchange tubes accounts for 20-50% of the cross-sectional area of the shell; preferably, the pipe diameter of each filtering pipe is 12mm-32mm, and the pipe diameter of each heat exchange pipe is 10mm-30 mm.
The utility model provides an among the tubular crystallizer, many heat exchange tubes and many filter tubes staggered arrangement preferably adopt triangle-shaped or rectangle dot matrix to arrange.
Preferably, the outer wall of the heat exchange tube is provided with heat exchange fins, so that the mass transfer and heat exchange area is increased.
Preferably, the shell consists of an upper end enclosure, a middle pipe and a lower end enclosure which are movably connected, and the heat exchange medium inlet is communicated with the heat exchange medium outlet through the space in the lower end enclosure, the heat exchange pipe and the space in the upper end enclosure.
Preferably, a liquid-solid interface detection device is arranged at the top end in the product melting chamber and is used for detecting the height of a solid-phase interface in the crystallization process. And when the liquid-solid interface detection equipment detects that the product melting chamber is filled with the solid-phase product, stopping feeding the raw materials, introducing a heating medium into the heating pipe to heat the crystallizer, and entering a melting and discharging stage.
Preferably, a liquid level height detection device is arranged at the bottom in the product melting chamber and used for detecting the liquid level height in the product melting chamber. And when the liquid level height detection equipment detects that all the liquid is extracted after melting, finishing the single intermittent operation.
Preferably, the pipeline connected with the raw material inlet, the wax product outlet and the liquid phase outlet is provided with an automatic control switch valve, and the automatic switching operation of the crystallization process is realized through the high linkage of a control system, a solid phase interface and a liquid level.
Preferably, the raw material inlet is communicated with a feeding precooler, and the liquid phase outlet is communicated with a vacuum-pumping system through a collecting tank. And (4) extracting the liquid-phase isoparaffin collected in the liquid-phase collection chamber by negative pressure.
The utility model provides a tubular crystallizer's application method does: firstly, a cooling medium is introduced through a heat exchange medium inlet 101, and the crystallizer is cooled through a heat exchange pipe 301 and then extracted through a pipeline 105. The material to be crystallized is introduced into the product melting chamber I from the raw material inlet 102, and the normal alkane therein is solidified and separated out due to cooling. After the product melting chamber I is filled with the liquid-solid mixed material, the liquid phase mainly containing isoparaffin at the upper layer enters the filter pipe 302, gradually enters the liquid phase collection chamber II through the filter pipe 302, is extracted through the liquid phase outlet 103 and is collected. And stopping feeding of the raw material inlet after the product melting chamber I is filled with the solid-phase product, introducing a heating medium through the heat exchange medium inlet 101 to heat the crystallizer, melting the solid-phase product in the product melting chamber I into a liquid phase, and collecting the liquid phase serving as the crystallized n-alkane product through the product outlet 104. Stopping extracting after all the liquid is extracted after melting, and finishing single intermittent operation.
The utility model provides an among the shell and tube crystallizer, crystallization separation/product melt accomplish in same casing space, the product melts the indoor. The liquid phase collecting chamber and the product melting chamber share one shell and are separated by a partition plate. And a plurality of filter pipes are arranged in the liquid phase collecting chamber, the open ends of the filter pipes are directly communicated with the crystallization separation/product melting chamber, and the other ends of the filter pipes are blocked. The aperture of the filter pipe is 0.1-100 microns, and the filter pipe penetrates through the side shell space to be used as a crystallization liquid phase collecting chamber and is connected with the liquid phase collecting pipe.
The second aspect, the utility model provides a continuous paraffin crystallization separator, by the parallelly connected setting of at least two foretell shell and tube type crystallizers.
The utility model provides a continuous paraffin crystallization separator's application method does: two or more shell-and-tube crystallizers provided by the novel device are arranged in parallel, and are subjected to linkage control through liquid-solid interface/liquid level detection signals and material inlet and outlet valve switching. For example, two tubular crystallizers are arranged in parallel, when the first crystallizer is used for cooling crystallization, the other second crystallizer is used for melting discharge; after the second crystallizer finishes melting and discharging, introducing a cooling medium into the second crystallizer to be in a standby state; and after the first crystallizer is filled with the solid-phase material, the feeding is switched to the second crystallizer, and meanwhile, the first crystallizer is filled with the heating material to melt and extract the product, so that the continuous operation of raw material feeding and product extraction is realized.
The following further describes a specific embodiment of the shell-and-tube crystallizer provided by the present invention with reference to the attached drawings. The present invention is not limited thereto.
Fig. 1 is a schematic structural diagram of a shell-and-tube crystallizer provided by the present invention. As shown in fig. 1, the shell-and-tube crystallizer is composed of an upper head 106, a middle shell and a lower head 107, and the upper head is connected with the middle shell and the middle shell are connected with the lower head through flanges. The space in the shell is divided into a product melting chamber I at the lower part and a liquid phase collecting chamber II at the upper part by a partition plate 100, a heat exchange tube 301 penetrates through the space in the shell, a filter tube 302 is arranged in the liquid phase collecting chamber, the top of the filter tube is closed, the bottom opening of the filter tube is communicated with the product melting chamber I, and a plurality of heat exchange tubes and a plurality of filter tubes are arranged in a staggered mode; the heat exchange medium inlet 101 and the heat exchange medium outlet 105 are respectively arranged at two ends of the shell and are communicated through the heat exchange pipe 301, the product melting chamber is provided with a raw material inlet 102 and a product outlet 104, and the lower part of the liquid phase collecting chamber is provided with a liquid phase outlet 103.
FIG. 2 is a schematic view of an arrangement of the filter tubes and heat exchange tubes in the product melting chamber. The filtering tubes 302 and the heat exchanging tubes 301 are arranged in a staggered manner at intervals and are respectively arranged in a rectangular lattice manner.
The present invention is further illustrated by the following examples. And the invention is not to be restricted thereby.
In the comparative examples and examples, the carbon number compositions of the raw hydrocarbon oil and the product were measured by gas chromatography analysis, and the enthalpy of phase change and melting range were measured by differential scanning calorimetry analysis.
Comparative example 1
Comparative example 1 adopts a conventional phase-change wax production method, namely, the raw material is cut in a fraction section, then a target fraction section is crystallized, and isoparaffin in the target fraction section is removed to obtain a phase-change wax product (reference CN 111100601A).
The raw material adopted is hydrogenated Fischer-Tropsch wax which is obtained from China petrochemical group company, Zhenhai division, and the main carbon number distribution of the hydrogenated Fischer-Tropsch wax is shown in Table 1, wherein the total normal carbon content is 86 wt%. The raw material is cut into different distillation sections, such as 300-330 ℃, 330-360 ℃, 360-390 ℃ and 390-420 ℃ by an ASTM standard real boiling point distillation device. The crystallization operation is carried out on the distillation section (the property is shown in table 2) with the temperature of 330-360 ℃, and a batch crystallization kettle is adopted for crystallization. Firstly, melting an oil product, slowly cooling to 32 ℃, solidifying part of raw materials into solid, taking out a liquid phase in the solid, slowly heating the solid phase until the temperature reaches 37 ℃, stabilizing for 1h, and obtaining a normal product after crystallization. The composition and enthalpy of phase change were analyzed. The normal phase product properties are shown in tables 3 and 4.
Example 1
Example 1 the same feed as in comparative example 1, namely the 330 c to 360 c fraction of hydrogenated fischer-tropsch wax (properties see table 2), was crystallized using the new crystallizer. The temperature of the product melting chamber is controlled to be 37 +/-0.5 ℃ by circulating water bath. The properties of the as-crystallized product are shown in tables 3 and 4.
As can be seen from tables 3 and 4, the utility model provides a normal paraffin content of the product obtained by the tubular crystallizer is higher, the enthalpy of phase change is higher, and the melting range is narrower.
TABLE 1 Fischer-Tropsch wax feed Properties
| Carbon number | Total carbon/%) | Normal carbon/%) | Isomeric carbon/%) | Carbon number | Total carbon/%) | Normal carbon/%) | Isomeric carbon/%) |
| C20 | 2.22 | 2.202 | 0.018 | C28 | 3.672 | 3.485 | 0.187 |
| C21 | 2.641 | 2.623 | 0.018 | C29 | 3.578 | 3.364 | 0.214 |
| C22 | 3.024 | 3.006 | 0.018 | C30 | 3.62 | 3.375 | 0.245 |
| C23 | 3.347 | 3.302 | 0.045 | C31 | 3.337 | 3.075 | 0.262 |
| C24 | 3.567 | 3.527 | 0.04 | C32 | 3.19 | 2.924 | 0.266 |
| C25 | 3.692 | 3.615 | 0.077 | C33 | 3.039 | 2.769 | 0.27 |
| C26 | 3.744 | 3.629 | 0.115 | C34 | 2.888 | 2.614 | 0.274 |
| C27 | 3.731 | 3.578 | 0.153 | C35 | 2.741 | 2.467 | 0.274 |
The content is mass percent.
TABLE 2330 deg.C-360 deg.C fraction Properties
| Carbon number | Mass fraction/% |
| C16 | 2.086 |
| C17 | 4.216 |
| C18 | 8.247 |
| C19 | 14.112 |
| C20 | 18.318 |
| C21 | 18.368 |
| C22 | 14.487 |
| C23 | 9.334 |
| C24 | 5.159 |
| C25 | 2.647 |
| C26 | 1.366 |
| Total of | 98.34 |
| Normal carbon | 83.5 |
TABLE 3 Properties of the as-crystallized product
TABLE 4 comparison of Normal product Properties
| Contrast item | Comparative example 1 | Example 1 |
| Enthalpy of phase change, J/g | 176 | 190 |
| Melting range, deg.C | 13 | 10 |
Claims (11)
1. A shell-and-tube crystallizer is characterized in that a space in a shell is divided into a product melting chamber (I) at the lower part and a liquid phase collecting chamber (II) at the upper part by a partition plate (100), a heat exchange tube (301) penetrates through the space in the shell, a filter tube (302) is arranged in the liquid phase collecting chamber, the top of the filter tube is closed, an opening at the bottom of the filter tube is communicated with the product melting chamber, and a plurality of heat exchange tubes and a plurality of filter tubes are arranged in a staggered mode; the heat exchange medium inlet (105) and the heat exchange medium outlet (101) are respectively arranged at two ends of the shell and are communicated through the heat exchange tubes, the product melting chamber is provided with a raw material inlet (102) and a wax product outlet (104), and the lower part of the liquid phase collecting chamber is provided with a liquid phase outlet (103).
2. A shell-and-tube crystallizer as in claim 1, characterized in that the filter tubes have a pore size of 0.1-100 microns.
3. A shell-and-tube crystallizer as in claim 2, wherein the filter tubes are selected from the group consisting of metal sintered tubes and ceramic membrane tubes.
4. A shell and tube crystallizer as claimed in claim 1, characterized in that the total cross-sectional area of the filter tubes accounts for 10% -30% of the cross-sectional area of the liquid phase collecting chamber, and the total cross-sectional area of the heat exchange tubes accounts for 20% -50% of the cross-sectional area of the shell; the pipe diameter of each filtering pipe is 12mm-32mm, and the pipe diameter of each heat exchange pipe is 10mm-30 mm.
5. A shell-and-tube crystallizer as recited in claim 1, wherein the outer walls of said heat exchange tubes are provided with heat exchange fins.
6. A shell and tube crystallizer as recited in claim 1, wherein said shell is composed of an upper head, a middle tube and a lower head which are movably connected, and said heat exchange medium inlet is communicated with the heat exchange medium outlet through the space in the lower head, the heat exchange tubes and the space in the upper head.
7. A shell-and-tube crystallizer as in claim 1, characterized in that the product melting chamber (i) is equipped with a liquid-solid interface detection device at its top end for detecting the solid-phase interface height during crystallization.
8. A shell-and-tube crystallizer as in claim 1, characterized in that a level detecting device is installed in the bottom of the product melting chamber (i) for detecting the level in the product melting chamber.
9. A shell and tube crystallizer as claimed in any one of claims 1 to 8, wherein automatic control valves are provided in the lines connecting the feed inlet, the wax product outlet and the liquid phase outlet, and are interlocked with the solid phase interface and liquid level height via a control system to effect automatic switching of the crystallization process.
10. A shell and tube crystallizer as claimed in any one of claims 1 to 8 wherein the feed inlet communicates with a feed precooler and the liquid phase outlet communicates with a vacuum pumping system via a collection tank.
11. A continuous paraffin crystallization separation apparatus, characterized in that at least two shell-and-tube crystallizers according to any one of claims 1 to 8 are arranged in parallel.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115970326A (en) * | 2023-02-08 | 2023-04-18 | 连云港铭磊科技有限公司 | High-purity crystallizer for acrylic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115970326A (en) * | 2023-02-08 | 2023-04-18 | 连云港铭磊科技有限公司 | High-purity crystallizer for acrylic acid |
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