CN115505055B - Method for reducing black polymer generation in carbon nine product - Google Patents
Method for reducing black polymer generation in carbon nine product Download PDFInfo
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- CN115505055B CN115505055B CN202110630163.8A CN202110630163A CN115505055B CN 115505055 B CN115505055 B CN 115505055B CN 202110630163 A CN202110630163 A CN 202110630163A CN 115505055 B CN115505055 B CN 115505055B
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 87
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229920000642 polymer Polymers 0.000 title claims abstract description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 65
- 238000002360 preparation method Methods 0.000 claims abstract description 54
- XESZUVZBAMCAEJ-UHFFFAOYSA-N 4-tert-butylcatechol Chemical compound CC(C)(C)C1=CC=C(O)C(O)=C1 XESZUVZBAMCAEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920001174 Diethylhydroxylamine Polymers 0.000 claims abstract description 25
- FVCOIAYSJZGECG-UHFFFAOYSA-N diethylhydroxylamine Chemical compound CCN(O)CC FVCOIAYSJZGECG-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000002347 injection Methods 0.000 claims abstract description 11
- 239000007924 injection Substances 0.000 claims abstract description 11
- 238000011049 filling Methods 0.000 claims description 27
- 238000010992 reflux Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 63
- 238000006116 polymerization reaction Methods 0.000 description 19
- BJEMXPVDXFSROA-UHFFFAOYSA-N 3-butylbenzene-1,2-diol Chemical group CCCCC1=CC=CC(O)=C1O BJEMXPVDXFSROA-UHFFFAOYSA-N 0.000 description 14
- 239000003112 inhibitor Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 150000001993 dienes Chemical class 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000005262 decarbonization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000686 essence Substances 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 235000010254 Jasminum officinale Nutrition 0.000 description 1
- 240000005385 Jasminum sambac Species 0.000 description 1
- 240000004277 Pelargonium radens Species 0.000 description 1
- 235000004789 Rosa xanthina Nutrition 0.000 description 1
- 241000109329 Rosa xanthina Species 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
- C08F2/40—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation using retarding agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F240/00—Copolymers of hydrocarbons and mineral oils, e.g. petroleum resins
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for reducing black polymer generation in a carbon nine product, which comprises the steps of injecting toluene solvent into a preparation tank, starting a centrifugal pump to circulate the toluene solvent, wherein the circulation time is more than 15 minutes, and finishing after finishing 1 working cycle; after circulation is completed, an electric heater is started to heat the toluene solvent, and after the toluene solvent temperature reaches 30-40 ℃, diethyl hydroxylamine and p-tert-butyl catechol are sequentially injected into a preparation tank, wherein the mass ratio of the diethyl hydroxylamine to the p-tert-butyl catechol to the toluene solvent is 5:3:12; starting an electric heater to heat the mixed liquid, controlling the temperature of the mixed liquid to be 30-45 ℃, starting a centrifugal pump to circulate the mixed liquid, and cooling to room temperature after the circulation time is more than 30 minutes and 2 working cycles are completed; and (3) sending the mixed liquid into an injection tank, starting a metering pump to inject the mixed liquid into the carbon nine product, and uniformly mixing to reduce the generation of black polymers in the carbon nine product.
Description
Technical Field
The invention relates to a method for reducing black polymer production in a carbon nine product, in particular to a method for reducing the content of black polymer by adding a polymerization inhibitor capable of slowing down or preventing diene polymerization in a carbon nine component, which aims to solve the technical problem that the black polymer affects the quality of the carbon nine product and belongs to the technical field of slowing down or preventing diene polymerization by adding the polymerization inhibitor.
Background
The derivative of the carbon nine product can be used as a blended spice of essences such as roses, iris, oranges, jasmine, pelargonium roseum and the like, and also can be independently used as a raw material of the carbon nine petroleum resin or as a raw material of solvent oil. With the rapid development of national economy in China, the consumption capability of the carbon nine products is increased year by year, although the carbon nine products in China are continuously increased, the requirements of downstream device production still cannot be met, the domestic carbon nine resins are insufficient in supply, especially the development of new technologies of the carbon nine products, and the use types of the carbon nine products are more and more. The carbon nine product in China is mainly prepared by taking crude gasoline as a byproduct of cracking ethylene as a raw material, and removing light components such as carbon five, carbon six-carbon eight and the like to obtain the carbon nine product. Since the carbon nine product contains dicyclopentadiene and polycycloalkene with active chemical properties, self polymerization and inter polymerization can easily occur, and particularly under the aerobic condition, the polymerization is more active, some granular or flocculent black substances are generated, the quality of the carbon nine product is influenced, and therefore, in the production and storage process of the carbon nine, proper polymerization inhibitor is required to be added to slow down or prevent the polymerization, and the polymerization inhibitor cannot influence the quality of the carbon nine derivative or the carbon nine petroleum resin product.
In the prior art for producing pyrolysis gasoline, raw material crude pyrolysis gasoline is treated, carbon five light components are removed by a decarbonization five tower of a prefractionation system, then the raw material crude pyrolysis gasoline enters a decarbonization nine tower, carbon six-carbon seven components are produced at the top, carbon eight-carbon nine components are produced at the bottom, the raw material is used as raw material for producing styrene by a styrene extraction (STED) technology, carbon nine products are produced by a carbon eight cutting unit, however, in the actual operation process, a small amount of black substances appear in the produced carbon nine products, and after long-time storage (about one week), the black is gradually increased, so that the quality of the carbon nine products is affected.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for reducing the content of black polymers in a carbon nine product, and a polymerization inhibitor capable of slowing down or preventing the polymerization of diolefins in the carbon nine component is used in the process, so that the method has the advantages of simple process, low added value mixture, stable process operation, simplicity, practicability and the like.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method of reducing black polymer production in a carbon nine product comprising the steps of:
(1) Filling: injecting a proper amount of toluene solvent into a preparation tank through a movable reciprocating pump, starting the centrifugal pump to circulate the toluene solvent in the preparation tank through a reflux return line, wherein the circulation time is 15 minutes or more, and the process is finished after 1 working cycle is completed;
(2) Heating: after the circulation of the step (1) is completed, an electric heater is started to heat the toluene solvent in the preparation tank, and the temperature of the toluene solvent in the preparation tank is controlled to be between 30 and 40 ℃;
(3) Mixing: the toluene solvent temperature in the step (2) reaches 30-40 ℃, and diethylhydroxylamine and p-tert-butylcatechol (TBC) are sequentially injected into a preparation tank, wherein the mass ratio of the diethylhydroxylamine to the p-tert-butylcatechol to the toluene solvent is 5:3:12;
(4) And (3) circulation: after the mixing in the step (3) is finished, an electric heater is started to heat the mixed liquid in the preparation tank, the temperature of the mixed liquid is controlled to be between 30 and 45 ℃, then a centrifugal pump is started to circulate the mixed liquid in the preparation tank through a reflux return line, the circulation time is 30 minutes or more, the mixing is finished after the completion of 2 working cycles, and the temperature of the mixed liquid is reduced to the room temperature;
(5) And (3) injection: after the circulation of the step (4) is completed, the mixed liquid is pumped into the filling tank through the centrifugal pump, when the liquid level in the filling tank reaches 50% -60%, the metering pump is started, the mixed liquid is injected into the carbon nine product after being pressurized, and the black polymer in the carbon nine product can be reduced after uniform mixing.
In the technical scheme, in the step (1), the purity of the toluene solvent is more than or equal to 99.9wt percent, and the toluene solvent can meet the requirements of national product standard and quality products.
In the technical scheme, in the step (1), when the centrifugal pump is started to circulate the toluene solvent, the suction pressure is 0.02-0.03 MPa (g), the discharge pressure is 0.15-0.2 MPa (g), the suction flow and the discharge flow are 500kg/h, the operating temperature is 40 ℃, and the lift is 20m.
In the technical scheme, in the step (2), an electric heater is started to heat the toluene solvent in the preparation tank, and the temperature is preferably controlled at 35+/-1 ℃.
In the above technical scheme, in the step (4), the electric heater is started to heat the mixed liquid in the preparation tank, and the temperature of the mixed liquid is preferably controlled to be 35+/-1 ℃.
In the technical scheme, in the step (4), when the centrifugal pump is started to circulate the mixed liquid in the preparation tank, the suction pressure is 0.02-0.03 MPa (g), the discharge pressure is 0.15-0.2 MPa (g), the suction flow and the discharge flow are 500kg/h, the operation temperature is 40 ℃, and the lift is 20m.
In the above technical scheme, in step (5), the operation conditions of the metering pump are as follows: the suction pressure is 0.02-0.03 MPa (g), the discharge pressure is 0.6-0.7 MPa (g), the suction flow is 4-6 kg/h, the discharge flow is 4-6 kg/h, and the normal temperature operation and the lift are 60m.
In the above technical solution, in the step (5), when the polymerization inhibitor is injected into the carbon nine product, it is required to continuously inject the polymerization inhibitor into the carbon nine product in the same amount per hour, and the polymerization inhibitor is injected into the carbon nine product in a ratio of 150 to 200 μg (mixed liquid)/g (carbon nine product).
The invention also provides a device for reducing the generation of black polymers in a carbon nine product, which comprises a preparation tank and a filling tank which are connected in sequence, and is characterized in that:
the preparation tank is provided with an inlet A, an outlet A1 and a circulating port A2, wherein: the inlet A is connected with a movable reciprocating pump, and the pump inlet of the movable reciprocating pump is connected with a device capable of providing toluene solvent, diethyl hydroxylamine and p-tert-butyl catechol; the outlet A1 is connected with a centrifugal pump, the outlet of the centrifugal pump is divided into two paths, a line I is connected with a circulating port A2, a line II is connected with a filling tank, and valves are respectively arranged on the line I and the line II;
the filling tank is provided with an inlet B and an outlet B, wherein: the inlet B is connected with a line II of the centrifugal pump; the outlet B is connected with a metering pump, and the pump outlet of the metering pump is connected with a carbon nine product pipeline.
In the above technical scheme, the outlet A1, the centrifugal pump, the line I and the circulation port A2 form a return line, and the substances in the preparation tank can circulate along the return line.
The reciprocating pump is a movable reciprocating pump, and the preparation tank and the corresponding pipeline are provided with electric tracing. (electric tracing is that an electric heater charges and heats a coil); the movable reciprocating pump, the centrifugal pump and the metering pump are all conventional and existing products (or equipment capable of achieving the same function) in the field of pumps.
The technical scheme of the invention has the advantages that: the materials used in the invention have low economic added value, are easy to obtain, and change waste into valuable.
Drawings
FIG. 1 is a schematic view of the overall structure of the device of the present invention;
wherein 1 is a preparation tank, 2 is a movable reciprocating pump, 3 is a centrifugal pump, 4 is a filling tank, and 5 is a metering pump.
Detailed Description
The following detailed description of the technical scheme of the present invention is provided, but the present invention is not limited to the following descriptions:
the invention provides a device for reducing black polymer generation in a carbon nine product, which comprises a preparation tank 1 and a filling tank 4 which are connected in sequence, as shown in figure 1:
the preparation tank 1 is provided with an inlet A, an outlet A1 and a circulating port A2, wherein: the inlet A is connected with a movable reciprocating pump 2, and the pump inlet of the movable reciprocating pump is connected with a device capable of providing toluene solvent, diethyl hydroxylamine and p-tert-butyl catechol; the outlet A1 is connected with a centrifugal pump 3, the outlet of the centrifugal pump is divided into two paths, a line I is connected with a circulating port A2, a line II is connected with a filling tank 4, and valves are respectively arranged on the line I and the line II;
the filling tank 4 is provided with an inlet B and an outlet B, wherein: the inlet B is connected with a line II of the centrifugal pump 3; the outlet B is connected with a metering pump 5, and the pump outlet of the metering pump is connected with a carbon nine product pipeline;
the outlet A1, the centrifugal pump, the line I and the circulating port A2 form a reflux return line, and substances in the preparation tank can circulate along the reflux return line.
The invention also provides a method for reducing the generation of black polymers in a carbon nine product, comprising the steps of:
(1) Filling: injecting a proper amount of toluene solvent into the preparation tank 1 through the movable reciprocating pump 2, starting the centrifugal pump 3 to circulate the toluene solvent in the preparation tank through a reflux return line, wherein the circulation time is 15 minutes or more, and the process is finished after 1 working cycle is completed;
(2) Heating: after the circulation of the step (1) is completed, an electric heater is started to heat the toluene solvent in the preparation tank, and the temperature of the toluene solvent in the preparation tank is controlled to be between 30 and 40 ℃;
(3) Mixing: the toluene solvent temperature in the step (2) reaches 30-40 ℃, and diethylhydroxylamine and p-tert-butylcatechol (TBC) are sequentially injected into a preparation tank, wherein the mass ratio of the diethylhydroxylamine to the p-tert-butylcatechol to the toluene solvent is 5:3:12;
(4) And (3) circulation: after the mixing in the step (3) is finished, an electric heater is started to heat the mixed liquid in the preparation tank, the temperature of the mixed liquid is controlled to be between 30 and 45 ℃, then a centrifugal pump is started to circulate the mixed liquid in the preparation tank through a reflux return line, the circulation time is 30 minutes or more, the mixing is finished after the completion of 2 working cycles, and the temperature of the mixed liquid is reduced to the room temperature;
(5) And (3) injection: after the circulation of the step (4) is completed, the mixed liquid is sent into the filling tank 4 through the centrifugal pump 3, when the liquid level in the filling tank reaches 50% -60%, the metering pump 5 is started, the mixed liquid is injected into the carbon nine product after pressurization, and the black polymer in the carbon nine product can be reduced after uniform mixing.
The invention is illustrated below with reference to specific examples.
In the following examples of the present invention, toluene purity was not less than 99.9wt%, satisfying the requirements of national product standards and quality.
Example 1:
a method of reducing black polymer production in a carbon nine product comprising the steps of:
(1) Filling: injecting a proper amount of toluene solvent into a preparation tank through a movable reciprocating pump, starting a centrifugal pump to circulate the toluene solvent in the preparation tank, wherein the circulation time is 15 minutes, and finishing the circulation after completing 1 time of work; when the centrifugal pump was turned on to circulate the toluene solvent, the suction pressure was 0.025MPa (g), the discharge pressure was 0.18MPa (g), the suction flow rate and the discharge flow rate were 500kg/h, the operating temperature was 40℃and the head was 20m.
(2) Heating: after the circulation of the step (1) is completed, an electric heater is started to heat the toluene solvent in the preparation tank, and the temperature of the toluene solvent in the preparation tank is controlled to be 35+/-1 ℃;
(3) Mixing: after the toluene solvent temperature in the step (2) reaches 35+/-1 ℃, sequentially injecting diethylhydroxylamine and p-tert-butylcatechol (TBC) into a preparation tank, wherein the mass ratio of the diethylhydroxylamine to the p-tert-butylcatechol to the toluene solvent is 5:3:12;
(4) And (3) circulation: after the mixing in the step (3) is finished, an electric heater is started to heat the mixed liquid in the preparation tank, the temperature of the mixed liquid is controlled to be 38+/-1 ℃, then a reciprocating pump is started to circulate the mixed liquid in the preparation tank, the circulation time is 30 minutes, the mixing is finished after the 2 working cycles are finished, and the temperature of the mixed liquid is reduced to the room temperature; when the centrifugal pump is started to circulate the mixed liquid in the preparation tank, the suction pressure is 0.025MPa (g), the discharge pressure is 0.18MPa (g), the suction flow and the discharge flow are 500kg/h, the operation temperature is 40 ℃, and the lift is 20m;
(5) And (3) injection: after the circulation of the step (4) is completed, the mixed liquid is sent into the filling tank (4) through the centrifugal pump (3), when the liquid level of the filling tank reaches 50% -60%, the metering pump (5) is started, the mixture is pressurized and then injected into the carbon nine product, and the black polymer in the carbon nine product can be reduced after the mixture is uniformly mixed; the metering pump has the following operation conditions: the suction pressure is 0.02-0.03 MPa (g), the discharge pressure is 0.6-0.7 MPa (g), the suction flow is 4-6 kg/h, the discharge flow is 4-6 kg/h, and the normal temperature operation and the lift are 60m;
when the mixed liquid is injected into the carbon nine product, continuous injection is required, the injection amount of the mixed liquid is the same every hour, the injection flow rate of the mixed liquid is 5kg/h, the injection flow rate of the carbon nine product is 25t/h, and the ratio of the mixed liquid to the carbon nine product is 200 mug (mixed liquid): 1g (carbon nine product).
In this example, after the mixed liquid was injected with the carbon nine product and mixed uniformly, no black material appeared in the case of 30 days of storage.
Comparative example 1:
under the condition of room temperature, diethyl hydroxylamine, para-Tertiary Butyl Catechol (TBC) and toluene are added into a preparation tank in batches according to the mass ratio of 5:3:12, the diethyl hydroxylamine, the para-Tertiary Butyl Catechol (TBC) and the toluene are fully mixed, a centrifugal pump is started for circulation, the circulation time and the circulation condition are the same as those of the step (4) of the embodiment 1, the mixed liquid is fed into the filling tank, and then the mixed liquid is continuously injected into a carbon nine product (the mixed solution with the same mass is injected every hour) through a metering pump, wherein the injection ratio is the same as that of the embodiment 1.
After the scheme is implemented, a small amount of p-tert-butyl catechol (TBC) is not completely dissolved, so that the polymerization inhibition effect of a carbon nine product is affected: after the mixed liquid is injected with the carbon nine product and uniformly mixed, the carbon nine product has a small amount of flocculent black substances under the condition of 8 days of storage.
Comparative example 2:
adding diethylhydroxylamine, p-tert-butylcatechol (TBC) and toluene into a preparation tank in batches according to the mass ratio of 5:3:12 at 25 ℃ to fully mix the three materials, and starting a centrifugal pump for circulation for 15 minutes (other circulation conditions are the same as those in the step (4) of the embodiment 1); the mixed liquid was fed into the filling tank, and then the mixed liquid was continuously injected into the carbon nine product (the same mass of the mixed solution was injected per hour) by the metering pump in the same ratio as in example 1.
After the scheme is implemented, a small amount of p-tert-butyl catechol (TBC) is not completely dissolved, so that the polymerization inhibition effect of a carbon nine product is affected: after the mixed liquid is injected into the carbon nine product and uniformly mixed, the carbon nine product has a small amount of flocculent black substances under the condition of 10 days of storage.
Comparative example 3:
at 40 ℃, diethyl hydroxylamine, para-Tertiary Butyl Catechol (TBC) and toluene are added into a preparation tank in batches according to the mass ratio of 1:1:8, so that the diethyl hydroxylamine, the para-Tertiary Butyl Catechol (TBC) and the toluene are fully mixed, a centrifugal pump is started for circulation, and the circulation time and the circulation condition are the same as those of the step (4) of the embodiment 1. The mixed liquid was fed into the filling tank, and then the mixed liquid was continuously injected into the carbon nine product (the same mass of the mixed solution was injected per hour) by the metering pump in the same ratio as in example 1.
In this example, after the carbon nine product was injected into the mixed liquid and mixed uniformly, a small amount of flocculent black material appeared on the carbon nine product in 15 days of storage.
Comparative example 4:
at 40 ℃, diethyl hydroxylamine, para-Tertiary Butyl Catechol (TBC) and toluene are added into a preparation tank in batches according to the mass ratio of 1:4:15, so that the diethyl hydroxylamine, the para-Tertiary Butyl Catechol (TBC) and the toluene are fully mixed, a centrifugal pump is started for circulation, and the circulation time and the circulation condition are the same as those of the step (4) of the embodiment 1. The mixed liquid was fed into the filling tank, and then the mixed liquid was continuously injected into the carbon nine product (the same mass of the mixed solution was injected per hour) by the metering pump in the same ratio as in example 1.
In this example, after the carbon nine product was injected into the mixed liquid and mixed uniformly, a small amount of flocculent black material appeared in the carbon nine product when stored for 25 days.
Comparative example 5:
at 40 ℃, diethyl hydroxylamine, para-Tertiary Butyl Catechol (TBC) and toluene are added into a preparation tank in batches according to the mass ratio of 1:1:3, so that the diethyl hydroxylamine, the para-Tertiary Butyl Catechol (TBC) and the toluene are fully mixed, a centrifugal pump is started for circulation, and the circulation time and the circulation condition are the same as those of the step (4) of the embodiment 1. The mixed liquid was fed into the filling tank, and then the mixed liquid was continuously injected into the carbon nine product (the same mass of the mixed solution was injected per hour) by the metering pump in the same ratio as in example 1.
In this example, after the carbon nine product was injected into the mixed liquid and mixed uniformly, a small amount of flocculent black material appeared in the carbon nine product when stored for 28 days.
From the above results, it can be seen that: the active components of diethylhydroxylamine and para-Tertiary Butyl Catechol (TBC) can effectively prevent or slow down the polymerization reaction of a carbon nine product, but the melting point of the para-Tertiary Butyl Catechol (TBC) is 52-57 ℃ and is solid at normal temperature, so that a sufficient amount of toluene solvent is needed to dissolve the para-Tertiary Butyl Catechol (TBC), otherwise, the para-tertiary butyl catechol is easy to crystallize, and the product quality is affected.
By combining the above factors, diethyl hydroxylamine, para-Tertiary Butyl Catechol (TBC) and toluene are added into a preparation tank in batches according to the mass ratio of 5:3:12 at the temperature of 30-40 ℃ so that the diethyl hydroxylamine, the para-Tertiary Butyl Catechol (TBC) and the toluene are fully mixed, a pump of a machine is started for circulation, the circulation time is ensured to be more than 30 minutes, and the mixed solution prepared under the condition can not only prevent or slow down the polymerization of a carbon nine product, but also reduce the energy consumption.
The foregoing examples are merely illustrative of the technical concept and technical features of the present invention, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made according to the essence of the present invention should be included in the scope of the present invention.
Claims (8)
1. A method for reducing black polymer production in a carbon nine product comprising the steps of:
(1) Filling: injecting a proper amount of toluene solvent into the preparation tank (1) through the movable reciprocating pump (2), starting the centrifugal pump (3) to circulate the toluene solvent in the preparation tank through the reflux return line, wherein the circulation time is 15 minutes or more, and the process is finished after 1 working cycle is completed;
(2) Heating: after the circulation of the step (1) is completed, an electric heater is started to heat the toluene solvent in the preparation tank, and the temperature of the toluene solvent in the preparation tank is controlled to be between 30 and 40 ℃;
(3) Mixing: the toluene solvent temperature in the step (2) reaches 30-40 ℃, and diethylhydroxylamine and p-tert-butylcatechol (TBC) are sequentially injected into a preparation tank, wherein the mass ratio of the diethylhydroxylamine to the p-tert-butylcatechol to the toluene solvent is 5:3:12;
(4) And (3) circulation: after the mixing in the step (3) is finished, an electric heater is started to heat the mixed liquid in the preparation tank, the temperature of the mixed liquid is controlled to be between 30 and 45 ℃, then a centrifugal pump is started to circulate the mixed liquid in the preparation tank through a reflux return line, the circulation time is 30 minutes or more, the mixing is finished after the completion of 2 working cycles, and the temperature of the mixed liquid is reduced to the room temperature;
(5) And (3) injection: after the circulation of the step (4) is completed, the mixed liquid is sent into the filling tank (4) through the centrifugal pump (3), when the liquid level in the filling tank reaches 50% -60%, the metering pump (5) is started, the mixed liquid is injected into the carbon nine product after pressurization, and the black polymer in the carbon nine product can be reduced after uniform mixing;
the method for reducing the generation of the black polymer in the carbon nine product is carried out in a device for reducing the generation of the black polymer in the carbon nine product, and the device for reducing the generation of the black polymer in the carbon nine product comprises a preparation tank (1) and a filling tank (4) which are connected in sequence, wherein:
the preparation tank (1) is provided with an inlet A, an outlet A1 and a circulating port A2, wherein: the inlet A is connected with a movable reciprocating pump (2), and the pump inlet of the movable reciprocating pump is connected with a device capable of providing toluene solvent, diethyl hydroxylamine and p-tert-butyl catechol; the outlet A1 is connected with a centrifugal pump (3), the outlet of the centrifugal pump is divided into two paths, a line I is connected with a circulating port A2, a line II is connected with a filling tank (4), and valves are respectively arranged on the line I and the line II;
the filling tank (4) is provided with an inlet B and an outlet B, wherein: the inlet B is connected with a line II of the centrifugal pump (3); the outlet B is connected with a metering pump (5), and the pump outlet of the metering pump is connected with a carbon nine product pipeline.
2. The method according to claim 1, characterized in that: in the step (1), when the centrifugal pump is started to circulate the toluene solvent, the suction pressure is 0.02-0.03 MPa (g), the discharge pressure is 0.15-0.2 MPa (g), the suction flow and the discharge flow are 500kg/h, the operating temperature is 40 ℃, and the lift is 20m.
3. The method according to claim 1, characterized in that: in the step (2), an electric heater is started to heat the toluene solvent in the preparation tank, and the temperature is controlled at 35+/-1 ℃.
4. The method according to claim 1, characterized in that: in the step (4), an electric heater is started to heat the mixed liquid in the preparation tank, and the temperature of the mixed liquid is controlled to be 35+/-1 ℃.
5. The method according to claim 1, characterized in that: in the step (4), when the centrifugal pump is started to circulate the mixed liquid in the preparation tank, the suction pressure is 0.02-0.03 MPa (g), the discharge pressure is 0.15-0.2 MPa (g), the suction flow and the discharge flow are 500kg/h, the operation temperature is 40 ℃, and the lift is 20m.
6. The method according to claim 1, characterized in that: in the step (5), the operation conditions of the metering pump are as follows: the suction pressure is 0.02-0.03 MPa (g), the discharge pressure is 0.6-0.7 MPa (g), the suction flow is 4-6 kg/h, the discharge flow is 4-6 kg/h, and the normal temperature operation and the lift are 60m.
7. The method according to claim 1, characterized in that: in the step (5), when the mixed liquid is injected into the carbon nine product, the mixed liquid is required to be continuously injected and the injection amount per hour is the same, and the mixed liquid is injected into the carbon nine product according to the ratio of the mixed liquid to the carbon nine product=150 to 200 μg/g.
8. The method according to claim 1, characterized in that: the outlet A1, the centrifugal pump, the line I and the circulating port A2 form a reflux return line, and substances in the preparation tank can circulate along the reflux return line.
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| CN101107274A (en) * | 2005-01-18 | 2008-01-16 | 丽川Ncc株式会社 | Polymerization inhibitor for 1,3-butadiene and a method of inhibiting polymerization of 1,3-butadiene by imputing thereof |
| CN101412663A (en) * | 2008-11-28 | 2009-04-22 | 江苏工业学院 | Preparation technique for polymerization inhibitor products |
| CN203393061U (en) * | 2013-08-15 | 2014-01-15 | 北京燕山玉龙石化工程有限公司 | Polymerization inhibitor adding system |
| CN209260018U (en) * | 2018-12-13 | 2019-08-16 | 南京扬子精细化工有限责任公司 | A kind of device reducing polymer content in cracking carbon nine |
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| CN101107274A (en) * | 2005-01-18 | 2008-01-16 | 丽川Ncc株式会社 | Polymerization inhibitor for 1,3-butadiene and a method of inhibiting polymerization of 1,3-butadiene by imputing thereof |
| CN101412663A (en) * | 2008-11-28 | 2009-04-22 | 江苏工业学院 | Preparation technique for polymerization inhibitor products |
| CN203393061U (en) * | 2013-08-15 | 2014-01-15 | 北京燕山玉龙石化工程有限公司 | Polymerization inhibitor adding system |
| CN209260018U (en) * | 2018-12-13 | 2019-08-16 | 南京扬子精细化工有限责任公司 | A kind of device reducing polymer content in cracking carbon nine |
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