CN103265974B - Device for refining heavy liquid paraffin continuously - Google Patents

Device for refining heavy liquid paraffin continuously Download PDF

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CN103265974B
CN103265974B CN201310235409.7A CN201310235409A CN103265974B CN 103265974 B CN103265974 B CN 103265974B CN 201310235409 A CN201310235409 A CN 201310235409A CN 103265974 B CN103265974 B CN 103265974B
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reaction
reaction tower
outlet
gas
inlet
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CN103265974A (en
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张大景
王欣
马青辉
杨景行
姜奎祥
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HEBEI DAJING DATANG CHEMICAL EQUIPMENT CO Ltd
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HEBEI DAJING DATANG CHEMICAL EQUIPMENT CO Ltd
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Abstract

The invention belongs to the technical field of heavy liquid paraffin refining, and particularly discloses a device for refining heavy liquid paraffin continuously. The main technical scheme is as follows: the device for refining heavy liquid paraffin continuously comprises a reaction tower, wherein the inside of the reaction tower is divided into a defoaming area and a reaction area; the top of the reaction tower is provided with a hydrogen chloride gas discharge opening; an outlet capable of controlling the flowing out of reactants or precipitates is formed at the bottom of the reaction tower; a hydrogen chloride gas inlet is formed at the side bottom of the reaction tower; a liquefied paraffin inlet and a softened water inlet are formed in the middle upper part of the reaction tower; a purified liquefied paraffin outlet is formed in the lower side part of the reaction tower; a gas-liquid separation mechanism is arranged between the top of the reaction tower and a tail gas treatment system; reaction liquid circulating ports communicated with a radiator are formed in the upper and lower parts of the reaction area of the reaction tower. By utilizing the device, impurities in the liquid paraffin can be separated completely, and the device is a closed-type circulating device and has the characteristic of environment friendliness.

Description

Device for continuously refining heavy liquid paraffin
Technical Field
The invention belongs to the technical field of heavy liquid paraffin refining processes, and particularly relates to a device for continuously refining heavy liquid paraffin, which is used for producing chlorinated paraffin-52.
Background
The chlorinated paraffin-52 is an important industrial raw material and is widely used in the industries of polyvinyl chloride, polyurethane, rubber and plastic, oil products and the like. The heavy liquid paraffin is a basic raw material for producing the chlorinated paraffin-52, contains 3-10 ppm of aromatic hydrocarbon, basic nitrogen, iron ions and a few thousandth of water impurities, and the impurities can generate colored groups after chlorination, so that the quality of the subsequently produced chlorinated paraffin-52 is greatly influenced, and the production of the chlorinated paraffin-52 is confused for a long time; therefore, effective removal of aromatic hydrocarbon, basic nitrogen and iron ions before the heavy liquid paraffin is put into chlorination reaction is the basic condition for ensuring the quality of chlorinated paraffin-52. The current method for treating the liquid paraffin comprises the following steps: physical standing precipitation, hydrochloric acid continuous washing treatment and chemical hydrogen chloride treatment. The device used in the method mostly adopts a reaction kettle or other reaction tanks with lower height, and the reaction of the liquid paraffin, water and hydrogen chloride gas is difficult to ensure in the reaction process of the reaction equipment, so that not only is the impurities in the liquid paraffin difficult to remove, but also more importantly, a large amount of bubbles are generated in the reaction, and the reaction kettle and the reaction tank are difficult to effectively prevent flooding, thereby causing blockage to the subsequent process or tail gas pipelines and influencing the production.
Disclosure of Invention
The invention aims to provide a device for continuously refining heavy liquid paraffin, which can remove aromatic hydrocarbon, alkaline nitrogen, iron ions and water thereof.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
1. the utility model provides a device of refining heavy liquid paraffin in succession which characterized in that: the reaction tower is internally divided into a defoaming area and a reaction area from top to bottom, the top of the reaction tower is provided with a hydrogen chloride gas discharge port, the bottom of the reaction area of the reaction tower is provided with an outlet capable of controlling the outflow of reactants or sediments, the lateral bottom of the reaction area is provided with a hydrogen chloride inlet, the middle upper part of the reaction area is provided with a liquefied paraffin inlet and a softened water inlet, and the lower lateral part of the reaction area is provided with a purified liquefied paraffin outlet; a gas-liquid separation mechanism is arranged between the top of the reaction tower and the tail gas treatment system, and an inlet, an exhaust port and a liquid outlet of the gas-liquid separation mechanism are respectively communicated with a hydrogen chloride gas exhaust port at the top of the reactor, a tail gas treatment system pipeline and a hydrogen chloride gas inlet; and the upper part and the lower part of the reaction zone of the reaction tower are provided with reaction liquid circulating ports communicated with the radiator.
Wherein, the liquid outlet of the gas-liquid separation mechanism is communicated with the opening at the lower side part of the reaction zone of the reaction tower.
2. A device for continuously refining heavy liquid paraffin comprises at least two stages of reaction towers which are internally divided into a defoaming area and a reaction area from top to bottom,
the bottom of the reaction zone of the reaction tower is provided with a reactant or precipitate outlet, the side bottom of the reaction zone is provided with a hydrogen chloride gas inlet, the middle upper part of the reaction zone is provided with a liquefied paraffin inlet, the lower side part of the reaction zone is provided with a purified liquefied paraffin outlet, and the top of the reaction tower is provided with a hydrogen chloride gas outlet;
a gas-liquid separation mechanism is arranged between the top of the reaction tower and the tail gas treatment system, and an inlet, an exhaust port and a liquid outlet of the gas-liquid separation mechanism are respectively communicated with a hydrogen chloride gas exhaust port at the top of the reaction tower, a tail gas treatment system pipeline and a hydrogen chloride gas inlet;
reaction liquid circulating ports communicated with the radiator are formed in the upper part and the lower part of the reaction zone of the reaction tower;
a softened water inlet is formed in the middle of the first-stage reaction tower in the reaction tower;
and inlets of the liquefied paraffin of other stages of reaction towers in the reactor are communicated with an outlet of the liquefied paraffin of the previous stage of reaction tower. And the inlet of the liquefied paraffin of the former stage reactor is higher than the inlet of the liquefied paraffin of the latter stage reaction tower, namely a potential difference is formed between the reaction towers.
Wherein,
the bottom of the reaction tower except the first-stage reaction tower is provided with a three-way mechanism at the outlet of reactants or sediments, one outlet of the three-way mechanism is a purified liquefied paraffin outlet, and the other outlet is a reactant or sediment outlet; a reactant or precipitate outlet arranged at the bottom of the reaction zone of the reaction tower is connected with the hydrochloric acid tank through a pipeline provided with a sight glass;
the tail gas treatment system is a second gas-liquid separation mechanism, an inlet of the gas-liquid separation mechanism is communicated with an exhaust port of the gas-liquid separation mechanism of the reaction tower, an exhaust port of the gas-liquid separation mechanism is communicated with the hydrogen chloride gas pipeline through a pipeline, and a liquid outlet of the gas-liquid separation mechanism is communicated with a reaction area of a last-stage reaction tower in the reaction tower.
Compared with the prior art, the device for continuously refining the heavy liquid paraffin has the following advantages: firstly, because the height of the reaction tower forming the device is about 10 meters, a reaction area and a defoaming area can be arranged in the reaction tower, so that the liquefied paraffin and hydrogen chloride gas input from the bottom side of the reaction tower can be fully reacted, the flooding phenomenon can be effectively avoided, and the continuous reaction is facilitated; secondly, because the reaction tower below the first-stage reaction tower forming the method and the device is not provided with a soft water inlet, the reaction in the reaction tower below the first stage can react residual water with a small amount of water left in the liquid paraffin and hydrogen chloride to generate high-concentration hydrochloric acid, and the high-concentration hydrochloric acid is separated from other impurity reaction products, so that the quality of the liquid paraffin is greatly improved; thirdly, a three-way valve mechanism provided with a sight glass is arranged at an outlet forming the liquid paraffin, namely the bottom of the reaction tower, so that the accurate control of the outflow of the sediment is facilitated; fourthly, the device is a closed circulating device, namely hydrogen chloride gas formed by the tail gas treatment system and liquid separated by the gas-liquid separation mechanism are finally circulated into the reaction tower, so that the device with the structure has the characteristic of environmental protection.
Drawings
FIG. 1 is a schematic view showing the structure of a continuous heavy liquid paraffin purification apparatus comprising a first-stage reaction column.
FIG. 2: is a schematic structural diagram of a continuous heavy liquid paraffin refining device composed of two stages of reaction towers.
Detailed Description
The structure and the operation principle of the device for continuously refining heavy liquid paraffin provided by the invention are further explained in detail with reference to the attached drawings as follows:
fig. 1 is a schematic structural diagram of a continuous refined heavy liquid paraffin constituted by a first-stage reaction tower according to the present invention. The device structurally comprises a reaction tower 3 which is internally divided into a defoaming area 1 and a reaction area 2 from top to bottom and has the height of about 10 meters, wherein the top of the reaction tower is provided with a hydrogen chloride gas outlet 41, the bottom of the reaction area of the reaction tower is provided with an outlet 5 which can control the outflow of reactants or sediments, the side bottom of the reaction area is provided with a hydrogen chloride inlet 7 communicated with a high-pressure hydrogen chloride gas source 6 through a pipeline, the middle upper part of the reaction area is provided with a liquid paraffin inlet 11 and a softened water inlet 12 which are respectively communicated with a liquid paraffin raw material source 9 and a softened water source 10 through pipelines, and the lower side part of the reaction area is provided with a purified liquefied paraffin outlet 13; a gas-liquid separation mechanism 151 is provided between the top of the reaction tower 3 and the off-gas treatment system 14, and an inlet 161, an exhaust port 171 and a liquid outlet 181 of the gas-liquid separation mechanism are respectively communicated with the hydrogen chloride gas outlet 41 at the top of the reaction tower, the off-gas treatment system 14 and the hydrogen chloride gas inlet 7 at the bottom of the reaction zone of the reaction tower; and reaction liquid upper and lower circulation ports 201 and 211 communicated with the radiator 191 are provided at the upper and lower sides of the reaction zone of the reaction tower.
The process for continuously refining the heavy liquid paraffin by using the device comprises the following steps:
continuously filling liquid paraffin, hydrogen chloride gas and softened water with the weight ratio of 1: 0.5-0.55: 0.01-0.02 into a reaction area in a reaction tower through a pipeline from a liquid paraffin inlet 11, a hydrogen chloride inlet 7 and a softened water inlet 12, reacting the softened water and the hydrogen chloride in the reaction tower to convert into hydrochloric acid, releasing heat energy to heat the liquid paraffin in the reaction tower, and further carrying out chemical reaction on the hydrochloric acid and aromatic hydrocarbon, basic nitrogen and iron ions contained in the liquid paraffin under the thermal action to generate reaction products such as benzyl chloride, dichlorotoluene, trichlorotoluene, benzenyl trichloride, ferric trichloride, pyridinium, quinolinium and the like; these reaction products each have a specific gravity of more than 1g/ml and are dissolved or mixed in hydrochloric acid having a specific gravity of more than 1.16g/ml to form a hydrochloric acid mixture, and the hydrochloric acid mixture is precipitated at the bottom of the reaction column toward the bottom of the liquid, thereby achieving a separation by layer from liquid paraffin having a specific gravity of less than 0.8g/ml, and the purified liquid paraffin is discharged through a liquefied paraffin outlet 13 provided at the bottom side of the reaction column.
In the refining process of the liquid paraffin, the excess heat generated by the reaction in the reaction tower is taken away by the radiators 191 arranged above and below the reaction zone; the excessive hydrogen chloride gas enters the gas-liquid separation mechanism 151 through an outlet via a pipeline, the separated liquid is communicated with a hydrogen chloride gas inlet 7 (or an inlet corresponding to the position) at the bottom of the reaction zone of the reaction tower via a pipeline and flows back to the reaction tower to participate in the reaction, and the primarily purified hydrogen chloride enters the tail gas treatment system 14 via an outlet 171 of the hydrogen chloride gas to be treated and then enters the hydrogen chloride absorption process.
In the above-described configuration, in order to prevent the hydrogen chloride hydrochloric acid liquid separated by the gas-liquid separation mechanism from entering the reaction tower through the hydrogen chloride gas inlet 7 and affecting the gas pipeline, a reflux port 221 is provided at the lower part of the reaction zone of the reaction tower, and the hydrogen chloride hydrochloric acid liquid separated by the gas-liquid separation mechanism enters the reaction tower through the reflux port 221 from the liquid outlet thereof.
Fig. 2 is a schematic structural diagram of a continuous refining heavy liquid paraffin composed of two stages of reaction towers according to the present invention. The device comprises a first-stage reaction tower and a second-stage reaction tower 23. Wherein the first-stage reaction tower has the same structure as the reaction tower 3 shown in fig. 1, the second-stage reaction tower 23 is also divided into a reaction area and a defoaming area, wherein a reactant or precipitate flow outlet 24 is arranged at the bottom of the reaction area, a hydrogen chloride inlet 25 communicated with a high-pressure hydrogen chloride gas source 6 through a pipeline is arranged at the bottom of the side of the reaction area, a liquefied paraffin inlet 26 communicated with a primarily purified liquid paraffin outlet 13 of the first-stage reaction tower through a pipeline is arranged at the middle upper part of the reaction area, a liquefied paraffin outlet 27 after secondary purification is arranged at the lower part of the reaction area, a second-stage gas-liquid separating mechanism 152 is arranged between a hydrogen chloride gas outlet 42 arranged at the top of the second-stage reaction tower 23 and a tail gas treatment system 14, an inlet 162, an exhaust outlet 172 and a liquid outlet 182 of the gas-liquid separating mechanism 152 are respectively connected with the hydrogen, The tail gas treatment system 14 is communicated with a hydrogen chloride gas inlet 25 at the bottom of the reaction zone of the reaction tower; the reaction zone of the secondary reaction tower is provided with upper and lower circulating ports 202 and 212 of reaction liquid communicated with the radiator 192; the inlet 11 of the first-stage reaction tower liquefied paraffin is higher than the inlet 26 of the second-stage reaction tower liquefied paraffin, so that a liquid level difference which is convenient for the liquid paraffin to enter the next-stage reaction tower exists between the front and the rear two stages of reaction towers.
The process for continuously refining the heavy liquid paraffin by utilizing the two-stage reaction tower comprises the following steps: the process steps of the first-stage reaction tower for refining the heavy liquid paraffin are consistent with the process of the reaction tower 3 in fig. 1, the primarily refined liquid paraffin flowing out of the liquefied paraffin outlet 13 of the first-stage reaction tower continuously flows into the reaction area of the first-stage reaction tower through the liquefied paraffin inlet 26 of the second-stage reaction tower, and the primarily refined liquid paraffin and hydrogen chloride gas entering the reaction area of the first-stage reaction tower through the high-pressure hydrogen chloride gas source 6 and the hydrogen chloride gas entering the reaction area of the reaction tower through the hydrogen chloride inlet 25 through the pipeline firstly form hydrochloric acid with the concentration of 36-38% with trace water in the primarily refined liquid paraffin, and the high-concentration hydrochloric acid continuously and the residual aromatic hydrocarbon, alkaline nitrogen and iron ions in the primarily refined liquid paraffin are subjected to chemical reaction again to generate reaction products such as benzyl chloride, dichlorotoluene, trichlorotoluene, benzenyl trichloride, ferric trichloride, pyridinium and quinoline salt; the specific gravity of the reaction products is more than 1g/ml, the reaction products are dissolved or mixed in hydrochloric acid with the specific gravity of more than 1.16g/ml to form a hydrochloric acid mixture, the hydrochloric acid mixture is precipitated at the bottom of the reaction tower to the bottom of the liquid, the liquid paraffin with the specific gravity of less than 0.8g/ml is separated by layers, the purified liquid paraffin flows out through a liquefied paraffin outlet 27 arranged at the bottom side part of the secondary reaction tower, and then the heavy liquid paraffin with higher purity can be obtained and enters the working procedure of producing chlorinated paraffin-52.
In the secondary refining process of the liquid paraffin passing through the secondary reaction kettle, the excess heat generated by the reaction in the secondary reaction tower is taken away by the radiators 192 arranged above and below the reaction zone; and the redundant wet hydrogen chloride gas enters a secondary gas-liquid separation mechanism 152 through a discharge port 42 arranged at the top of the secondary reaction kettle by a pipeline, the separated liquid is communicated with a hydrogen chloride gas inlet 7 at the bottom of the reaction area of the secondary reaction tower by a pipeline and flows back to the reaction tower to participate in the reaction, and the primarily purified hydrogen chloride enters a tail gas treatment system 14 from an outlet 172 of the hydrogen chloride gas through a pipeline to be treated and then enters a hydrogen chloride absorption process.
In the above-mentioned structure, in order to prevent the hydrogen chloride hydrochloric acid liquid separated by the secondary gas-liquid separation mechanism from entering the reaction tower from the hydrogen chloride gas inlet 25 and affecting the gas pipeline, a reflux port 222 is provided at the lower side of the reaction zone of the reaction tower, and the hydrogen chloride hydrochloric acid liquid separated by the gas-liquid separation mechanism enters the reaction tower from the liquid outlet thereof through the reflux port 222.
The device for continuously refining the heavy liquid paraffin can be provided with the number of reaction towers according to the requirement, the reaction tower may be composed of two stages as shown in FIG. 2, or may be composed of three, four or more stages connected in series after the two stages as shown in FIG. 2, and each stage of reaction tower is provided with a hydrogen chloride gas inlet communicated with a hydrogen chloride gas source and an inlet and an outlet of liquid paraffin, the outlet of the liquid paraffin of the previous stage of reaction tower is communicated with the inlet of the liquid paraffin of the next stage of reaction tower to form serial connection, the top of the added reaction tower is provided with a gas-liquid separation mechanism connected with a tail gas treatment system, the liquid outlet and the gas outlet of the separation mechanism are respectively communicated with the hydrogen chloride inlet of the reaction tower and the tail gas treatment system, so that the liquid paraffin purified by the previous stage reaction kettle is further purified to improve the quality of the liquid paraffin.
Because the reaction impurity content in the liquid paraffin can be greatly reduced after the purification of the first-stage reaction tower, a three-way mechanism 29 (as shown in fig. 2) is arranged at the outlet of the reactant or the precipitate at the bottom of other reaction towers except the first-stage reaction tower, a horizontal outlet 30 of the three-way mechanism is arranged as an outlet for purifying the liquefied paraffin, a vertical outlet 31 of the three-way mechanism is an outlet for the reactant or the precipitate, and a sight glass 33 is arranged on a pipeline connecting the outlet of the reactant or the precipitate at the bottom of the three-way mechanism and a hydrochloric acid tank 32. The removal condition of the reaction sediment can be observed through the sight glass, namely, the switch 34 is closed after the sediment is removed, so that the purified liquid paraffin flows out through the horizontal outlet, and the removal precision of the sediment can be improved.
The liquid paraffin described in this patent application is a normal straight-chain paraffin with a carbon chain length of 13-17, and the molecular weight of 184-240, which is a product from petroleum.

Claims (6)

1. The utility model provides a device of refining heavy liquid paraffin in succession which characterized in that: the reaction tower is internally divided into a defoaming area and a reaction area from top to bottom, the top of the reaction tower is provided with a hydrogen chloride gas outlet, the bottom of the reaction area of the reaction tower is provided with an outlet capable of controlling the outflow of reactants or sediments, the lateral bottom of the reaction area is provided with a hydrogen chloride inlet, the middle upper part of the reaction area is provided with a liquefied paraffin inlet and a softened water inlet, and the lower lateral part of the reaction area is provided with a purified liquefied paraffin outlet; a gas-liquid separation mechanism is arranged between the top of the reaction tower and the tail gas treatment system, and an inlet, an exhaust port and a liquid outlet of the gas-liquid separation mechanism are respectively communicated with a hydrogen chloride gas exhaust port at the top of the reactor, a tail gas treatment system pipeline and a hydrogen chloride gas inlet; and the upper part and the lower part of the reaction zone of the reaction tower are provided with reaction liquid circulating ports communicated with the radiator.
2. The apparatus for continuously refining heavy liquid paraffin according to claim 1, wherein: and a liquid outlet of the gas-liquid separation mechanism is communicated with a port at the lower side part of the reaction zone of the reaction tower.
3. The utility model provides a device of refining heavy liquid paraffin in succession which characterized in that: comprises at least two reaction towers which are internally divided into a defoaming area and a reaction area up and down,
the bottom of the reaction zone of the reaction tower is provided with a reactant or precipitate outlet, the side bottom of the reaction zone is provided with a hydrogen chloride gas inlet, the middle upper part of the reaction zone is provided with a liquefied paraffin inlet, the lower side part of the reaction zone is provided with a purified liquefied paraffin outlet, and the top of the reaction tower is provided with a hydrogen chloride gas outlet;
a gas-liquid separation mechanism is arranged between the top of the reaction tower and the tail gas treatment system, and an inlet, an exhaust port and a liquid outlet of the gas-liquid separation mechanism are respectively communicated with a hydrogen chloride gas exhaust port at the top of the reaction tower, a tail gas treatment system pipeline and a hydrogen chloride gas inlet;
reaction liquid circulating ports communicated with the radiator are formed in the upper part and the lower part of the reaction zone of the reaction tower;
a softened water inlet is formed in the middle of the first-stage reaction tower in the reaction tower;
inlets of the liquefied paraffin of other stages of reaction towers in the reactor are communicated with an outlet of the liquefied paraffin of the previous stage of reaction tower; and the inlet of the liquefied paraffin of the former stage reactor is higher than the inlet of the liquefied paraffin of the latter stage reaction tower, namely a potential difference is formed between the reaction towers.
4. The apparatus for continuously refining heavy liquid paraffin according to claim 3, wherein: and the outlets of the reactants or the sediments at the bottoms of other reaction towers except the first-stage reaction tower are provided with a three-way mechanism, one outlet of the three-way mechanism is a purified liquefied paraffin outlet, and the other outlet of the three-way mechanism is a reactant or sediment outlet.
5. The apparatus for continuously refining heavy liquid paraffin according to claim 3 or 4, wherein: and a reactant or precipitate outlet arranged at the bottom of the reaction zone of the reaction tower is connected with the hydrochloric acid tank through a pipeline provided with a sight glass.
6. The apparatus for continuously refining heavy liquid paraffin according to claim 3, wherein: the tail gas treatment system is a second gas-liquid separation mechanism, an inlet of the gas-liquid separation mechanism is communicated with an exhaust port of the gas-liquid separation mechanism of the reaction tower, an exhaust port of the gas-liquid separation mechanism is communicated with the hydrogen chloride gas pipeline through a pipeline, and a liquid outlet of the gas-liquid separation mechanism is communicated with a reaction area of a last-stage reaction tower in the reaction tower.
CN201310235409.7A 2013-06-14 2013-06-14 Device for refining heavy liquid paraffin continuously Active CN103265974B (en)

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CN103265974B true CN103265974B (en) 2014-12-10

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106833743A (en) * 2017-03-30 2017-06-13 河北大景大搪化工设备有限公司 A kind of serialization purifies the device of Paraffin liquid heavy

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB496273A (en) * 1937-05-25 1938-11-25 Universal Oil Prod Co Process for the production of paraffin hydrocarbons
CN102888245A (en) * 2012-09-19 2013-01-23 沁阳市海世鸿工贸有限责任公司 Method and device for refining liquid paraffin
CN203284376U (en) * 2013-06-14 2013-11-13 河北大景大搪化工设备有限公司 Device for refining heavy liquid paraffin continuously

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB496273A (en) * 1937-05-25 1938-11-25 Universal Oil Prod Co Process for the production of paraffin hydrocarbons
CN102888245A (en) * 2012-09-19 2013-01-23 沁阳市海世鸿工贸有限责任公司 Method and device for refining liquid paraffin
CN203284376U (en) * 2013-06-14 2013-11-13 河北大景大搪化工设备有限公司 Device for refining heavy liquid paraffin continuously

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