Ring body impurity removal system and hydrolysate loop line separation system

By using water washing, physical adsorption, and distillation processes in the cyclic impurity removal system, the problems of impurities and odors in the cyclic compounds have been solved, thereby improving the purity of the cyclic compounds and reducing production costs.

CN223561500UActive Publication Date: 2025-11-18HESHENG SILICON (JIAXING) CO LTD
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Patent Information

Application Number
CN202422739371.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-11-11
Publication Date
2025-11-18
Estimated Expiration
2034-11-11

AI Technical Summary

Technical Problem

Existing ring separation technology results in the presence of D4, D5 and light component impurities in the rings. Direct sale is not economically viable, and recycling the rings into the hydrolysate tank increases the consumption of cracking steam, leading to resource waste and high production costs.

Method used

A cyclic impurity removal system is adopted, including an impurity removal device, an odor removal device, and a distillation device. Impurities and odors in the cyclic material are removed through water washing, physical adsorption, and distillation processes, thereby improving the purity of the cyclic material.

Benefits of technology

It improved the production quality of the ring, reduced resource waste, lowered production costs, reduced steam consumption, and enhanced economic efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a ring body impurity removal system and a hydrolysate loop line separation system, the ring body impurity removal system comprises an impurity removal device, an odor removal device and a rectification device which are arranged in sequence, the impurity removal device is suitable for removing impurities in a ring body through water washing, the odor removal device is suitable for removing impurities in the ring body through a physical adsorbent, and the rectification device is suitable for rectifying the ring body; and condensing the gas phase obtained by rectification to obtain a ring body. The ring body impurity removal system provided by the utility model can remove impurities such as acid, alkali and salt in a ring body, reduce the generation of peculiar smell of a product, separate cyclic volatile methylsiloxane (D3, D4 and D5) as far as possible, and perform external extraction on a small part of residual decamethylcyclopentasiloxane D5 and residues, so that the cracking process of the ring body is reduced, the steam consumption is reduced, and the production cost is reduced.
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Description

Technical Field

[0001] This application relates to the field of chemical organosilicon production technology, and in particular to a ring-type impurity removal system and a hydrolysate ring-type separation system. Background Technology

[0002] Circulating separation is a process that effectively separates cyclic compounds (such as cyclosiloxanes) from linear compounds (such as linear siloxanes) in organosilicon hydrolysates using distillation separation technology. The linear compounds are sent to the downstream workshop to produce low-viscosity 107 adhesive, while the cyclic compounds are cooled by circulating water and sent to the hydrolysis workshop's hydrolysate storage tank, then to the pyrolysis process to produce cyclic compounds, which are then subjected to cyclic distillation to produce cyclic volatile methylsiloxanes (DMC / D4, D5) products, or directly packaged and sold. However, existing circulating separation technology has the following drawbacks: After a period of operation, sampling and testing of the cyclic compounds in the workshop revealed that the majority contained D4 (75%-80%) and D5 (20%-55%), with some hydroxyl-terminated small linear compounds and other light component impurities. Direct sale is not economically efficient, and recycling the cyclic compounds into the hydrolysate tank and then sending them to the pyrolysis process increases pyrolysis steam consumption, resulting in resource waste and increased production costs.

[0003] With overcapacity among organosilicon monomer manufacturers and fierce market competition, manufacturers are constantly expanding downstream products, making good use of by-products, adjusting product structure, and carrying out technological transformations in energy conservation and consumption reduction to reduce production costs. Summary of the Invention

[0004] One objective of this application is to improve the quality of cyclic compound production and reduce impurities in small filaments and other light components.

[0005] Another objective of this application is to reduce waste of recycled resources and lower production costs.

[0006] To achieve the above objectives, the technical solution adopted in this application is as follows: a ring body impurity removal system, comprising an impurity removal device, an odor removal device, and a distillation device arranged sequentially. The impurity removal device is adapted to remove impurities in the ring body by washing with water. The odor removal device is adapted to remove impurities in the ring body by using a physical adsorbent. The distillation device is adapted to distill the ring body and condense the gas phase obtained by distillation to obtain the ring body.

[0007] As a preferred embodiment, the impurity removal device includes a refining vessel and a separator arranged in sequence. The refining vessel is adapted to remove impurities from the ring body by stirring and washing, and the separator is adapted to allow the top of the ring body to overflow and the bottom to settle and drain.

[0008] As a preferred, the deodorizing device comprises a decoloring kettle, a filter and a third buffer tank arranged in sequence, the decoloring kettle is suitable for adding adsorbent material to adsorb impurities in the ring body, the filter is suitable for circulating and filtering out impurities and residual adsorbent material in the ring body, and the third buffer tank is suitable for settling the ring body after removing impurities and odor.

[0009] As a preferred, the ring body is pumped from the top of the layer separator to the decoloring kettle, the deodorizing agent is added from the top of the decoloring kettle, the impurities in the ring body are adsorbed by the adsorbent material, and then the ring body passes through the filter to remove the adsorbent material, and the ring body is sent to the third buffer tank after passing through the filter.

[0010] As a preferred, the rectifying device comprises a rectifying tower, a third heat exchanger, a third condenser and a storage tank arranged in sequence, the rectifying tower is suitable for further purifying the ring body, the third heat exchanger is suitable for transferring exchanged heat to the rectifying tower, and the third condenser enables the gaseous ring body to be converted into condensed liquid and stored in the storage tank.

[0011] As a preferred, the ring body in the third buffer tank is pumped to the rectifying tower by a production pump, the target product is distilled from the top of the rectifying tower, condensed by the third condenser and stored in the storage tank, and the impurities are produced from the bottom of the rectifying tower by the production pump.

[0012] As a preferred, a hydrolysate ring line separation system comprises a separation device, a refining device and the ring body impurity removal system, and the ring body separated from the hydrolysate by the separation device and the refining device is pumped into the ring body impurity removal system for impurity removal.

[0013] As a preferred, the separation device comprises a separation tower, a first heat exchanger, a first condenser and a first buffer tank arranged in sequence, the ring body separated from the hydrolysate overflows from the top of the separation tower, is condensed by the first condenser and then input into the first buffer tank, and is pumped to the refining kettle after settling in the first buffer tank.

[0014] As a preferred, the refining device comprises a refining tower, a second heat exchanger, a second condenser and a second buffer tank arranged in sequence, the line body containing a small amount of ring body separated from the hydrolysate is pumped from the bottom of the separation tower to the refining tower, the residual ring body overflows from the top of the refining tower, is condensed by the second condenser and then input into the second buffer tank, and is pumped to the refining kettle after settling in the second buffer tank.

[0015] Compared with the prior art, the application has the beneficial effects that:

[0016] (1) The impurity removal device in the application can remove impurities such as acid, alkali and salt in the ring body through the refining kettle, reduce the acid value of the ring body, and reduce the influence of the subsequent rectification and temperature rise on the product quality.

[0017] (2) The odor removal device in the application can reduce the generation of peculiar smell of the product by adding diatomite and activated carbon in the decoloring kettle for adsorption and impurity removal.

[0018] (3) The filtered ring body in the application enters the rectification tower, and the condenser can separate as much as possible the cyclic volatile methylsiloxane (D3, D4, D5) from the top of the tower, and the remaining small part of D5 and the residue are taken out through the tower kettle, so that the entering into the cracking process is reduced, the steam consumption is reduced, and the production cost is reduced. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 It is a schematic diagram of the ring body impurity removal system of the utility model.

[0020] Figure 2 It is a schematic diagram of the hydrolysate ring line separation system in the embodiment.

[0021] In the figure: 10, separation device; 11, separation tower; 12, first condenser; 13, first buffer tank; 14, first heat exchanger; 20, refining device; 21, refining tower; 22, second condenser; 23, second buffer tank; 24, second heat exchanger; 30, impurity removal device; 31, refining kettle; 32, layering device; 40, odor removal device; 41, decoloring kettle; 42, filter; 43, third buffer tank; 50, rectification device; 51, rectification tower; 52, third heat exchanger; 53, third condenser; 54, storage tank. DETAILED DESCRIPTION

[0022] In the following, the application will be further described in conjunction with specific embodiments, and it should be noted that the following described embodiments or technical features can be combined in any manner to form new embodiments without conflict.

[0023] In the description of the application, it should be noted that for orientation words, such as terms "center", "transverse", "longitudinal", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate the orientation and positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the application and simplifying the description, and cannot be understood as indicating or implying that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and cannot be understood as limiting the specific protection scope of the application.

[0024] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application are used to distinguish similar objects, and do not necessarily have to be used to describe a specific order or sequence.

[0025] The terms "include" and "have" and any variations thereof in the specification and claims of the present application are intended to cover non-exclusive inclusion, for example, a process, method, system, product or device including a series of steps or units does not have to be limited to only those steps or units clearly listed, but can include other steps or units not clearly listed or inherent to these processes, methods, products or devices.

[0026] In the prior art hydrolyzate ring line separation rectification process, part of the low components and hydroxyl-terminated small rings are pumped to the vent system by vacuum, and part of them are condensed by the overhead condenser and then sent to the reflux tank to the cracking process to be converted into ring materials, which has high energy consumption and high production cost.

[0027] To solve the problems in the prior art, the present application proposes a ring impurity removal system, which refines the part of the ring and then sends it to the ring storage tank of the ring rectification process for separation.

[0028] As shown in Figure 1 The ring impurity removal system proposed by the present application includes a decontamination device 30, a deodorization device 40 and a rectification device 50 arranged in sequence, the ring to be treated is delivered to the decontamination device 30 by a production pump, the decontamination device 30 removes impurities in the ring by water washing, the ring after decontamination is delivered to the deodorization device 40, the deodorization device 40 continues to remove impurities in the ring by physical adsorption, the ring after the deodorization device 40 is delivered to the rectification device 50 to further remove impurities by rectification process, and the gas phase obtained by rectification is condensed to obtain the product ring.

[0029] In some embodiments, the decontamination device 30 includes a refining kettle 31 and a layer separator 32 arranged in sequence, the ring in the refining kettle 31 can remove impurities such as acid, alkali and salt in the ring by stirring water washing, reduce the acid value of the ring, and reduce the influence of acid value enrichment after subsequent rectification and temperature rise on product quality, the ring containing water is separated in the layer separator 32, the upper layer is the ring, and the lower layer is water, the ring overflows from the top of the layer separator 32 and is delivered to the deodorization device 40 by a pump, and the water is settled and discharged from the bottom of the layer separator 32, so as to improve the purity and quality of the ring by the decontamination device 30.

[0030] In some embodiments, the deodorization device 40 comprises a decoloring kettle 41, a filter 42 and a third buffer tank 43 arranged in sequence, the decoloring kettle 41 is suitable for adding adsorbent material so that impurities in the ring body in the decoloring kettle, especially odor impurities, are adsorbed by the adsorbent material, the ring body output from the decoloring kettle 41 enters the filter 42 so as to separate the adsorbent material from the ring body, and the separated ring body enters the third buffer tank 43 for sedimentation, and the water and impurities at the bottom of the third buffer tank 43 are discharged through the bottom, and the ring body above is transported to the rectification device 50 for rectification. The deodorization device 40 mainly utilizes the physical adsorption of the adsorbent material to remove odor impurities in the ring body. The adsorbent material can be selected from one or more of diatomite and activated carbon. Since the odor is generated by the aggregation of impurities such as hydrocarbon impurities after rectification, which affects the product quality, the diatomite and activated carbon with high cost performance and strong adsorption capacity are selected for effective adsorption, and thus the deodorizing agent used in the deodorization device 40 is diatomite and activated carbon with high cost performance and strong adsorption capacity.

[0031] In some embodiments, since the acid, alkali and salt impurities in the ring body can change the properties of the functional groups of the activated carbon and diatomite required for ring body deodorization, thereby affecting the adsorption capacity of the activated carbon, the ring body first needs to enter the impurity removal device 30 in the ring body impurity removal system to remove the acid, alkali and salt impurities therein, and then the impurity-removed ring body is transported to the deodorization device 40 for adsorption and impurity removal by diatomite and activated carbon, so as to effectively reduce the generation of product odor while not affecting the quality of the ring body output.

[0032] In some embodiments, the filter 42 used in the deodorization device 40 is a plate and frame with simple structure, convenient operation and easy maintenance, and the ring body can repeatedly enter the decoloring kettle 41 for further filtration treatment after preliminary filtration by the plate and frame, until the ring body is colorless and transparent in appearance observed through the sight glass, and then the ring body is sent into the third buffer tank 43, so as to realize further purification of the ring body.

[0033] In some embodiments, the rectification device 50 comprises a rectification tower 51, a third heat exchanger 52, a third condenser 53 and a storage tank 54 arranged in sequence, the ring body in the third buffer tank 43 is pumped to the rectification tower 51 by a production pump, the gas phase distilled from the top of the rectification tower 51 is condensed by the third condenser 53 and then transported to the storage tank 54, and the remaining small amount of D5 and residues are discharged through the tower kettle, so as to reduce the entry into the cracking process and the steam consumption and reduce the production cost.

[0034] In some embodiments, the ring body impurity removal system also needs to be used in cooperation with the hydrolysate ring line separation system, such as Figure 2As shown, the hydrolysate ring separation system includes a separation device 10 and a purification device 20 arranged in sequence. The separation device 10 is suitable for separating the hydrolysate rings and lines, and the purification device 20 is used to further obtain high-purity rings. The rings obtained by the separation of the hydrolysate through the separation device 10 and the purification device 20 are pumped to the ring impurity removal system for further impurity removal.

[0035] In some embodiments, the separation device 10 in the hydrolysate loop separation system includes a separation tower 11, a first heat exchanger 14, a first condenser 12, and a first buffer tank 13 arranged in sequence. The gaseous ring separated from the hydrolysate overflows from the top of the separation tower 11, is condensed by the first condenser 12, and is then fed into the first buffer tank 13. After settling in the first buffer tank 13, the ring is pumped to the refining kettle 31 for further impurity removal.

[0036] In some embodiments, the refining device 20 in the hydrolysate loop separation system includes a refining tower 21, a second heat exchanger 24, a second condenser 22, and a second buffer tank 23 arranged sequentially. The hydrolysate with a small amount of residual rings is pumped from the bottom of the separation tower 11 to the refining tower 21. The residual rings overflow from the top of the refining tower 21, are then condensed by the second condenser 22, and fed into the second buffer tank 23. After settling in the second buffer tank 23, they are pumped to the refining kettle 31 for further impurity removal.

[0037] like Figures 1-2 As shown, specific embodiments of the hydrolysate ring separation and ring impurity removal system in this application are as follows:

[0038] (1) The hydrolysate enters the separation tower 11. The rings with lower boiling points are distilled off from the top of the separation tower 11, condensed by the first condenser 12, and then fed into the first buffer tank 13. The line at the bottom of the separation tower 11 still contains a small amount of rings. The line discharged from the separation tower 11 is fed into the refining tower 21. The remaining rings are distilled off from the top of the refining tower 21, condensed by the second condenser 22, and then fed into the second buffer tank 23.

[0039] (2) The rings in the first buffer tank 13 and the second buffer tank 23 are fed into the refining kettle 31. The impurities such as acids, alkalis and salts in the rings are removed by stirring and washing. Then the rings are sent to the separator 32 for separation. The rings are pumped from the top of the separator 32 to the decolorizing kettle 41. Activated carbon, diatomaceous earth and other adsorbent materials are added to the decolorizing kettle 41. The colored impurities and / or odorous impurities in the rings are adsorbed by the adsorbent materials. Then the rings are passed through the filter 42 to remove the adsorbent materials. After the rings are observed to be colorless and transparent through the sight glass, they are sent to the third buffer tank 43.

[0040] (3) The ring body in the third buffer tank 43 is transported to the rectification tower 51 by the extraction pump, and the target products D3, D4 and D5 are distilled from the top of the rectification tower 51 and stored in the storage tank 54 after being condensed by the third condenser 53, and the impurities are extracted from the bottom of the rectification tower 51 by the extraction pump.

[0041] As shown in the specific embodiment of the ring body impurity removal system proposed for the above embodiment, the present application further proposes a specific operation step of the ring body impurity removal system: Figure 1

[0042] S10, the ring body separated by the hydrolysate ring line is sent to the refining kettle 31, the ring body feed is 2m 3 , and a proper amount of pure water is added into the refining kettle 31 for stirring for 2h, and then the ring body is sent to the layer separator 32 for settlement and drainage;

[0043] S20, the ring body overflows from the top of the layer separator 32, is transported to the decolorizing kettle 41 by the extraction pump, and the feed is 2m 3 , stirring is started, and a proper amount of activated carbon and diatomite is added into the top of the decolorizing kettle 41, and stirring is performed for 2h;

[0044] S30, the stirring is stopped, the discharge valve at the bottom of the decolorizing kettle 41 is opened, the ring body is transported into the plate and frame filter 42 by the extraction pump for circular filtration, and after the ring body is observed to be colorless and transparent in appearance, it is sent to the third buffer tank 43 of the ring body;

[0045] S40, the third buffer tank 43 is settled and drained, and then the target product is transported to the rectification tower 51 for rectification, and after being separated by heating, it is sent to the storage tank 54, and the remaining small part of D5 and the residue are extracted from the tower kettle of the rectification tower 51 by the extraction pump.

[0046] The ring body impurity removal system proposed in the present application, after the hydrolysate enters the ring line separation device 10, the ring body condensed and extracted from the top of the refining tower 21 is sent to the refining kettle 31, and by stirring and washing with water, the residual acid, alkali, salt and other impurities in the ring body can be effectively removed, the acid value of the ring body is reduced, and the influence of the acid value enrichment after subsequent rectification and heating on the product quality is reduced.

[0047] Further, the ring body further enters the ring body layer separator 32 for water removal, the upper part of the ring body in the layer separator 32 is transported to the decolorizing kettle 41 by the extraction pump, activated carbon and / or diatomite are added into the decolorizing kettle 41 to remove impurities and adsorb the peculiar smell of the ring body, and after stirring, the ring body is subjected to plate and frame circular filtration, and the ring body with impurities and peculiar smell removed is sent to the third buffer tank 43.

[0048] ​Further, the filtered ring body enters the third buffer tank 43 for sedimentation, the water and impurities separated at the bottom are drained for treatment, and the ring body is continuously pumped to the rectification column 51 for rectification. The gas phase at the top of the column is condensed to obtain D3, D4 and D5, which are sent to the storage tank 54. The remaining small amount of D5 and residues are collected from the bottom of the rectification column 51, thereby solving the problem of poor economic benefits of direct sale of ring body products, reducing the consumption of cracking steam, avoiding resource waste, reducing production costs, and reducing the production costs.

[0049] The present application first removes most of the acid, alkali and salt impurities in the ring body by stirring water washing, and then removes the impurities and odors in the ring body by physical adsorption of the odor removal agent, thereby effectively reducing the generation of odors in the ring body. Finally, further impurities are removed by rectification, which helps to evaporate as much as possible pure D3, D4 and D5 from the top of the column.

[0050] The above describes the basic principles, main features and advantages of the present application. Those skilled in the art should understand that the present application is not limited to the above embodiments, and the above embodiments and descriptions are only the principles of the present application. Without departing from the spirit and scope of the present application, various changes and improvements can be made to the present application, and these changes and improvements all fall within the scope of the claimed present application. The scope of protection claimed by the present application is defined by the appended claims and their equivalents.

Claims

1. A ring-shaped impurity removal system, characterized in that, The system comprises a decontamination device, a deodorization device and a rectification device arranged in sequence, the decontamination device is adapted to remove impurities in the ring body by water washing, the deodorization device is adapted to remove impurities in the ring body by physical adsorbent, and the rectification device is adapted to rectify the ring body and condense the gas phase obtained by rectification to obtain the ring body.

2. The system of claim 1, wherein, The decontamination device comprises a refining kettle and a separator arranged in sequence, the refining kettle is adapted to remove impurities in the ring body by stirring water washing, and the separator is adapted to overflow the ring body at the top and to settle and drain water at the bottom.

3. The system of claim 2, wherein the ring body is configured to rotate about the axis of rotation. The deodorization device comprises a decoloring kettle, a filter and a third buffer tank arranged in sequence, the decoloring kettle is adapted to add adsorbent to remove impurities in the ring body in the kettle, the filter is adapted to remove impurities and residual adsorbent in the ring body by circulation filtration, and the third buffer tank is adapted to settle and remove the ring body after removal of impurities and odor.

4. The system of claim 3, wherein the ring body is configured to rotate about the axis of rotation. The ring body is pumped from the top of the separator to the decoloring kettle, the deodorizing agent is added from the top of the decoloring kettle, the impurities in the ring body are adsorbed by the adsorbent, and then the ring body passes through the filter to remove the adsorbent, and the ring body passes through the filter and is sent to the third buffer tank.

5. The system of claim 3, wherein the ring body is made of a material selected from the group consisting of: stainless steel, titanium, and a polymer. 5 The rectification device comprises a rectification tower, a third heat exchanger, a third condenser and a storage tank arranged in sequence, the rectification tower is adapted to further purify the ring body, the third heat exchanger is adapted to transfer heat to the rectification tower, and the third condenser is adapted to convert the gaseous ring body into condensed liquid and store it in the storage tank.

6. The system of claim 5, wherein the ring body is configured to rotate about the axis of rotation. The ring body in the third buffer tank is pumped to the rectification tower by a production pump, the target product is distilled from the top of the rectification tower, condensed by the third condenser and stored in the storage tank, and the impurities are produced from the bottom of the rectification tower by the production pump.

7. A hydrolysate loop separation system characterized by, The system comprises a separation device, a refining device and the ring body decontamination system of any one of claims 1-6, the ring body separated by the separation device and the refining device from the hydrolysate is pumped into the ring body decontamination system for decontamination.

8. The hydrolysate loop separation system of claim 7, wherein, The decontamination device comprises a refining kettle and a separator arranged in sequence, the refining kettle is adapted to remove impurities in the ring body by stirring water washing, and the separator is adapted to overflow the ring body at the top and to settle and drain water at the bottom.

9. The hydrolysate loop separation system of claim 8, wherein, The separation device comprises a separation tower, a first heat exchanger, a first condenser and a first buffer tank arranged in sequence, the ring body separated from the hydrolysate is overflowed from the top of the separation tower, condensed by the first condenser and input into the first buffer tank, and pumped to the refining kettle after settling in the first buffer tank.

10. The hydrolysate loop separation system of claim 9, wherein, The refining device comprises a refining tower, a second heat exchanger, a second condenser and a second buffer tank arranged in sequence, the linear body containing a small amount of ring body separated from the hydrolysate is pumped from the bottom of the separation tower to the refining tower, the residual ring body is overflowed from the top of the refining tower, condensed by the second condenser and input into the second buffer tank, and pumped to the refining kettle after settling in the second buffer tank.