CN112940155A - Preparation process of petroleum resin with high reaction rate and low softening point - Google Patents
Preparation process of petroleum resin with high reaction rate and low softening point Download PDFInfo
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- CN112940155A CN112940155A CN202110079236.9A CN202110079236A CN112940155A CN 112940155 A CN112940155 A CN 112940155A CN 202110079236 A CN202110079236 A CN 202110079236A CN 112940155 A CN112940155 A CN 112940155A
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- 239000011347 resin Substances 0.000 title claims abstract description 57
- 229920005989 resin Polymers 0.000 title claims abstract description 57
- 239000003208 petroleum Substances 0.000 title claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 152
- 239000001257 hydrogen Substances 0.000 claims abstract description 101
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 101
- 239000002994 raw material Substances 0.000 claims abstract description 99
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 91
- 238000007667 floating Methods 0.000 claims abstract description 44
- 239000011261 inert gas Substances 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 230000009471 action Effects 0.000 claims abstract description 9
- 238000007493 shaping process Methods 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 24
- 238000007789 sealing Methods 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 14
- 150000002431 hydrogen Chemical class 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 8
- 239000012466 permeate Substances 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000012719 thermal polymerization Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 239000013013 elastic material Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 abstract description 9
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract description 9
- 229930195735 unsaturated hydrocarbon Natural products 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 description 9
- 230000001070 adhesive effect Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 238000004901 spalling Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 229930195734 saturated hydrocarbon Natural products 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000004831 Hot glue Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000005574 cross-species transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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
- C08F8/00—Chemical modification by after-treatment
- C08F8/04—Reduction, e.g. hydrogenation
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a process for preparing petroleum resin with high reaction rate and low softening point, which belongs to the technical field of resin preparation, and the process for preparing the petroleum resin with high reaction rate and low softening point comprises the steps of forming a large number of bubbles in a hydrogenation raw material under inert gas through the operation of hydrogen-containing pretreatment, reducing the density of the hydrogenation raw material to ensure that the internal porosity of the hydrogenation raw material is relatively large, and enabling hydrogen to enter the hydrogenation raw material more easily, so that the hydrogenation raw material can fully react with the hydrogen during the hydrogenation reaction, the content of unsaturated hydrocarbon in the petroleum resin is effectively ensured to be eliminated, increasing the hydrogen amount in the hydrogenation raw material with low density through the action of an upper floating ball, enabling the inside and the outside of the hydrogenation raw material to simultaneously react during the hydrogenation reaction, obviously improving the reaction efficiency of the hydrogenation reaction, and effectively avoiding incomplete reaction of the hydrogenation raw material on the inner side, the amount of unsaturated olefin is obviously reduced, so that the softening point of the unsaturated olefin is effectively reduced, and the application range is expanded.
Description
Technical Field
The invention relates to the technical field of resin preparation, in particular to a preparation process of petroleum resin with high reaction rate and low softening point.
Background
In recent years, the expansion of markets and consumption of hot melt adhesives, pressure-sensitive adhesives, road marking paints, rubbers, inks and the like has driven the development of petroleum resin industry. The traditional preparation method of the petroleum resin comprises a catalytic method and a thermal polymerization method, the petroleum resin produced by the catalytic polymerization method has narrow molecular weight distribution, better solubility in a solvent and smaller smell, is widely applied in the fields of adhesives, road marking paints, rubber, printing ink and the like, and can basically meet the requirements of customers in terms of performance; production of petroleum resin by thermal polymerization: simple process, less investment in equipment, no need of catalyst and no generation of waste water and waste residue.
However, in the process of producing petroleum resin by the traditional thermal polymerization method, the softening point of the produced resin is high, the viscosity is high, the compatibility is not good due to the high content of unsaturated olefin and high reaction activity, so that the application of the resin is limited, and the defects of the resin are more prominent particularly when the resin is applied to an adhesive. The petroleum resin is used as an important component in the adhesive except for the main elastomer, and the performance of the petroleum resin directly influences the performance and the application range of the adhesive. If the compatibility of the petroleum resin and the elastomer of the glue is poor, the wettability of the glue is poor; the resin has high viscosity, influences the permeability of the adhesive to an adherend, deteriorates the initial viscosity and the fluidity of the adhesive, is difficult to coat and cannot achieve the purpose of fast and firm bonding; the softening point of the resin is high, the low-temperature resistance of the adhesive is poor, the adhesive is easy to cure at low temperature, and the bonding strength is low, so that the use of the adhesive in cold winter is hindered.
In the prior art, the content of unsaturated olefin is usually reduced by hydrogenation, but hydrogen is difficult to completely contact with unsaturated olefin in the hydrogenation reaction process, so that partial unsaturated olefin still exists, and the effect of reducing the softening point of a resin finished product is not obvious.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a petroleum resin preparation process with high reaction rate and low softening point, which can form a large amount of bubbles in a hydrogenation raw material under inert gas through the operation of hydrogen-containing pretreatment, reduce the density of the hydrogenation raw material to ensure that the internal porosity of the hydrogenation raw material is relatively large and hydrogen can enter the hydrogenation raw material more easily, so that the hydrogenation reaction can be more sufficiently reacted with the hydrogen, thereby effectively ensuring the elimination of the content of unsaturated hydrocarbon in the petroleum resin, increase the hydrogen content in the low-density hydrogenation raw material through the action of an upper floating ball, ensure that the inside and the outside of the hydrogenation raw material can simultaneously react during the hydrogenation reaction, obviously improve the reaction efficiency of the hydrogenation reaction, effectively avoid the incomplete reaction of the hydrogenation raw material at the inner side and obviously reduce the amount of the unsaturated olefin, thereby effectively reducing the softening point and expanding the application range.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A preparation process of petroleum resin with high reaction rate and low softening point comprises the following steps:
s1, distilling a product obtained after the thermal polymerization reaction to obtain molten basic petroleum resin;
s2, mixing and diluting the basic petroleum resin with a hydrogenation solvent, and uniformly stirring to obtain a hydrogenation raw material;
s3, introducing the hydrogenation raw material into a transfer case for hydrogen-containing pretreatment, and then conveying the product subjected to hydrogen-containing pretreatment to a hydrogenation reactor containing a nickel catalyst for hydrogenation reaction;
and S4, removing the hydrogenation solvent after the hydrogenation reaction is finished, and obtaining the petroleum resin with low softening point.
Further, the mixing volume ratio of the base petroleum resin and the hydrogenation solvent in the S2 is 1: 2-5, the hydrogenation solvent is a saturated hydrocarbon solvent.
Further, the hydrogen-containing pretreatment specifically comprises the following operations:
s31, firstly, introducing the hydrogenation raw material into a transfer box;
s32, controlling a sealing pressure plate in the transfer box to move towards the liquid level of the hydrogenation raw material, then introducing inert gas into the interior through a gas inlet on the sealing pressure plate, wherein the inert gas permeates into the hydrogenation raw material to form a large number of bubbles inside, so that the density of the hydrogenation raw material is reduced, and the internal porosity of the hydrogenation raw material is relatively large, so that hydrogen can easily enter the interior, and the hydrogen can be fully reacted with hydrogen during hydrogenation reaction, thereby effectively ensuring to eliminate the content of unsaturated hydrocarbons in petroleum resin, further effectively reducing the softening point of the petroleum resin, and expanding the application range;
s331, opening the gas inlet, overflowing part of the inert gas, then filling hydrogen into the interior through the gas inlet, and permeating part of the hydrogen into the low-density hydrogenation raw material, so that the contact between the hydrogen and the hydrogenation raw material is obviously improved and the reaction completeness is improved compared with the hydrogenation reaction which is carried out in a separation mode of the hydrogenation raw material and the hydrogen in the prior art;
s332, the upper floating ball in the transfer box is heated under the action of the high-temperature hydrogenation raw material, and the hydrogen in the transfer box overflows and permeates into the hydrogenation raw material from the inner side.
Furthermore, the total amount of the hydrogen filled in the S331 and the hydrogen in the floating ball is greater than the total amount of the hydrogen required by the hydrogenation reaction, and the exceeding amount is not greater than 1/5 of the total amount of the required hydrogen, so that on one hand, the influence on the hydrogenation reaction caused by incomplete overflow of the hydrogen in the floating ball is effectively prevented, and on the other hand, more hydrogen effectively ensures that the hydrogenation reaction of the hydrogenation raw material and the hydrogen is more complete.
Furthermore, the transfer box comprises a box body, the right lower end of the box body is fixedly connected with a discharge hole, a sealing pressure plate with an air inlet is in interference fit with the inner wall of the box body, and the upper floating ball is fixedly connected to the inner bottom end of the box body.
Furthermore, the sealing pressure plate is positioned at the position of 3-4cm above the upper surface of the hydrogenation raw material, and provides a certain space for gas which enters the hydrogenation raw material and overflows, so that the situation of excessive gas spalling is not easy to occur.
Furthermore, the plurality of upper floating balls are different in height and are uniformly dispersed in the box body, the highest upper floating ball is positioned 5-10cm below the upper surface of the hydrogenation raw material, so that the plurality of air floating balls are dispersed in the hydrogenation raw material, and after heated hydrogen in the hydrogenation raw material overflows, the heated hydrogen can be uniformly dispersed into the hydrogenation raw material from the inner side, so that the hydrogenation reaction is more complete.
Furthermore, go up the floater including with box bottom fixed connection's flexible stay cord and fixed connection the gas floater on flexible stay cord, the inside hydrogen that has compression state that fills of gas floater, the compression multiple is no longer than 2 times, compressed hydrogen effectively guarantees that it can the rapid expansion spill over, makes the efficiency improvement of holding hydrogen preliminary treatment.
Furthermore, the gas floating ball comprises an upper shaping end, a lower gas outlet end fixedly connected to the lower end of the upper shaping end and a lower gas outlet end fixedly connected to the inner top end of the upper shaping end, the upper end of the flexible pull rope fixedly penetrates through the middle of the flexible pull rope and is fixedly connected with the lower gas outlet end, hydrogen is located in a space formed by the upper shaping end and the flexible pull rope, and a plurality of uniformly distributed pre-breaking sheets are embedded inside the flexible pull rope.
Furthermore, the upper shaping end is made of hard materials, the pre-broken thin sheet is made of elastic materials, the thickness of the pre-broken thin sheet is not more than half of the thickness, so that hydrogen is heated to expand under the action of the high-temperature hydrogenation raw material, the pre-broken thin sheet is preferentially cracked, and the hydrogen in the pre-broken thin sheet can overflow to the inner side of the hydrogenation raw material, so that the use effect of the pre-broken thin sheet is achieved.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) through the operation of hydrogen-containing pretreatment, on one hand, under the inert gas, a large amount of bubbles can be formed in the hydrogenation raw material, the density of the hydrogenation raw material is reduced, the internal porosity of the hydrogenation raw material is relatively large, hydrogen can easily enter the hydrogenation raw material, so that the hydrogenation reaction can be carried out more fully to react with the hydrogen, the content of unsaturated hydrocarbon in petroleum resin is effectively eliminated, on the other hand, the hydrogen amount can be increased in the low-density hydrogenation raw material through the action of the upper floating ball, the hydrogenation raw material can simultaneously react inside and outside during the hydrogenation reaction, the reaction efficiency of the hydrogenation reaction is remarkably improved, the condition that the reaction of the hydrogenation raw material on the inner side is easy to be incomplete is effectively avoided, the amount of unsaturated olefin is remarkably reduced, the softening point of the hydrogenation raw material is effectively reduced, and the.
(2) The sealing press plate in the transfer box is controlled to move towards the liquid level of the hydrogenation raw material, then inert gas is introduced into the interior through the gas inlet on the sealing press plate, the inert gas permeates into the hydrogenation raw material to form a large amount of bubbles in the interior, the density of the hydrogenation raw material is reduced, and the porosity of the interior of the hydrogenation raw material is relatively large, so that hydrogen can enter the interior of the hydrogenation raw material more easily, the hydrogenation reaction can be carried out more sufficiently, the content of unsaturated hydrocarbon in petroleum resin is effectively eliminated, the softening point of the petroleum resin is effectively reduced, and the application range is expanded.
(3) The gas inlet is opened, part of the inert gas overflows, then hydrogen is filled into the interior of the gas inlet, and part of the hydrogen permeates into the low-density hydrogenation raw material, so that the contact between the hydrogen and the hydrogenation raw material is obviously improved and the reaction completeness is improved compared with the hydrogenation reaction which is carried out in a separation mode of the hydrogenation raw material and the hydrogen in the prior art;
(4) the total amount of the hydrogen filled in the S331 and the hydrogen in the floating ball is larger than the total amount of the hydrogen needed by the hydrogenation reaction, and the exceeding amount is not larger than 1/5 of the total amount of the needed hydrogen, so that on one hand, the influence on the hydrogenation reaction caused by incomplete overflow of the hydrogen in the floating ball is effectively prevented, and on the other hand, more hydrogen effectively ensures that the hydrogenation reaction of the hydrogenation raw material and the hydrogen is more complete.
(5) The transfer box comprises a box body, a discharge port is fixedly connected to the right lower end of the box body, a sealing press plate with an air inlet is in interference fit with the inner wall of the box body, a plurality of upper floating balls are fixedly connected to the inner bottom end of the box body, and the sealing press plate is located at the position 3-4cm away from the upper surface of the hydrogenation raw material and provides a certain space for gas overflowing from the hydrogenation raw material, so that excessive gas spalling is not easy to occur.
(6) The plurality of upper floating balls are different in height and are uniformly dispersed in the box body, the highest upper floating ball is positioned 5-10cm below the upper surface of the hydrogenation raw material, so that the plurality of air floating balls are dispersed in the hydrogenation raw material, and after heated internal hydrogen overflows, the heated internal hydrogen can be uniformly dispersed into the hydrogenation raw material from the inner side, so that the hydrogenation reaction is more complete.
(7) The upper floating ball comprises a flexible pull rope fixedly connected with the bottom end in the box body and an air floating ball fixedly connected with the flexible pull rope, the interior of the air floating ball is filled with compressed hydrogen, the compression multiple is not more than 2 times, the compressed hydrogen effectively ensures that the compressed hydrogen can rapidly expand and overflow, so that the efficiency of hydrogen pretreatment is improved, the air floating ball comprises an upper shaping end, a lower air outlet end fixedly connected with the lower end of the upper shaping end and fixedly connected with the inner top end of the upper shaping end, the upper end part of the flexible pull rope fixedly penetrates through the middle part and is fixedly connected with the lower air outlet end, the hydrogen is positioned in a space enclosed by the upper shaping end and the lower air outlet end, a plurality of uniformly distributed pre-broken sheets are embedded in the air floating ball, the upper shaping end is made of hard materials, the pre-broken sheets are made of elastic materials, the thickness of the pre-, the pre-broken thin sheet is preferentially cracked, so that hydrogen in the pre-broken thin sheet can overflow to the inner side of the hydrogenation raw material, and the use effect of the hydrogenation raw material is improved.
Drawings
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is a schematic structural view of a section of a transfer case of the present invention;
FIG. 3 is a schematic structural view of the upper buoyant ball portion of the present invention;
FIG. 4 is a schematic structural view of the hydrogen gas in the buoyant spheres of the present invention when expanded after heating.
The reference numbers in the figures illustrate:
the device comprises a box body 1, a discharge hole 21, an air inlet 22, a sealing pressure plate 3, a flexible pull rope 4, an air floating ball 5, an upper shaping end 51, a lower air outlet end 52 and a pre-broken sheet 6.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; but not all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, a process for preparing petroleum resin with high reaction rate and low softening point comprises the following steps:
s1, distilling a product obtained after the thermal polymerization reaction to obtain molten basic petroleum resin;
s2, mixing and diluting the basic petroleum resin with a hydrogenation solvent, and uniformly stirring to obtain a hydrogenation raw material;
s3, introducing the hydrogenation raw material into a transfer case for hydrogen-containing pretreatment, and then conveying the product subjected to hydrogen-containing pretreatment to a hydrogenation reactor containing a nickel catalyst for hydrogenation reaction;
the specific operation of hydrogen-containing pretreatment is as follows:
s31, firstly, introducing the hydrogenation raw material into a transfer box;
s32, controlling a sealing pressure plate in the transfer box to move towards the liquid level of the hydrogenation raw material, introducing inert gas into the interior through a gas inlet 22 on the sealing pressure plate, wherein the inert gas permeates into the hydrogenation raw material to form a large number of bubbles inside, so that the density of the hydrogenation raw material is reduced, and the internal porosity of the hydrogenation raw material is relatively large, so that hydrogen can easily enter the interior, and the hydrogenation reaction can be fully reacted with hydrogen, thereby effectively ensuring the elimination of the content of unsaturated hydrocarbons in petroleum resin, further effectively reducing the softening point of the petroleum resin, and expanding the application range;
s331, opening the gas inlet 22, overflowing part of the inert gas, then filling hydrogen into the interior through the gas inlet 22, and permeating part of the hydrogen into the low-density hydrogenation raw material, so that the contact between the hydrogen and the hydrogenation raw material is obviously improved and the reaction completeness is improved compared with the hydrogenation reaction which is carried out in a way that the hydrogenation raw material and the hydrogen are separated in the prior art;
s332, the upper floating ball in the transfer box is heated under the action of the high-temperature hydrogenation raw material, and the hydrogen in the transfer box overflows and permeates into the hydrogenation raw material from the inner side.
And S4, removing the hydrogenation solvent after the hydrogenation reaction is finished, and obtaining the petroleum resin with low softening point.
The mixing volume ratio of the basic petroleum resin and the hydrogenation solvent in the S2 is 1: 2-5, the hydrogenation solvent is a saturated hydrocarbon solvent, the total amount of the hydrogen filled in the S331 and the hydrogen in the floating ball is greater than the total amount of the hydrogen required by the hydrogenation reaction, and the excessive amount is not greater than 1/5 of the total amount of the required hydrogen, so that on one hand, the influence on the hydrogenation reaction caused by incomplete overflow of the hydrogen in the floating ball is effectively prevented, and on the other hand, more hydrogen effectively ensures that the hydrogenation reaction of the hydrogenation raw material and the hydrogen is more complete;
referring to fig. 2, the transfer box includes a box body 1, a discharge port 21 is fixedly connected to the right lower end of the box body 1, a sealing press plate 3 with an air inlet 22 is in interference fit with the inner wall of the box body 1, a plurality of floating balls are fixedly connected to the inner bottom end of the box body 1, the sealing press plate 3 is located at 3-4cm of the upper surface of the hydrogenation raw material to provide a certain space for the gas which enters the hydrogenation raw material and overflows, so that excessive gas spalling is not likely to occur, the plurality of floating balls are different in height and are uniformly dispersed in the box body 1, the highest floating ball is located 5-10cm below the upper surface of the hydrogenation raw material, the plurality of floating balls 5 are dispersed in the hydrogenation raw material, and after the heated hydrogen inside overflows, the hydrogen can be uniformly dispersed in the hydrogenation raw material from the inner side, so that the hydrogenation reaction is more complete.
The upper floating ball comprises a flexible pull rope 4 fixedly connected with the inner bottom end of the box body 1 and an air floating ball 5 fixedly connected with the flexible pull rope 4, the air floating ball 5 is filled with compressed hydrogen, the compression multiple is not more than 2, the compressed hydrogen effectively ensures that the compressed hydrogen can rapidly expand and overflow, and the efficiency of hydrogen pretreatment is improved, please refer to fig. 3, the air floating ball 5 comprises an upper shaping end 51, a lower end 53 fixedly connected with the lower end 51 of the upper shaping end and a lower air outlet end 52 fixedly connected with the inner top end of the upper shaping end 51, the upper end of the flexible pull rope 4 fixedly penetrates through the middle part of the upper shaping end 53 and is fixedly connected with the lower air outlet end 52, the hydrogen is positioned in a space enclosed by the upper shaping ends 51 and 53, a plurality of pre-broken sheets 6 are uniformly distributed and embedded in the upper shaping end 51, the upper shaping end 51 is made of hard material, the upper shaping end 53 and the pre, referring to fig. 4, under the action of the high-temperature hydrogenation raw material, hydrogen expands under heat, so that the pre-broken thin sheet 6 preferentially cracks, and the hydrogen inside the pre-broken thin sheet can overflow to the inner side of the hydrogenation raw material, thereby achieving the using effect.
Through the operation of hydrogen-containing pretreatment, on one hand, under the inert gas, a large amount of bubbles can be formed in the hydrogenation raw material, the density of the hydrogenation raw material is reduced, the internal porosity of the hydrogenation raw material is relatively large, hydrogen can easily enter the hydrogenation raw material, so that the hydrogenation reaction can be carried out more fully to react with the hydrogen, the content of unsaturated hydrocarbon in petroleum resin is effectively eliminated, on the other hand, the hydrogen amount can be increased in the low-density hydrogenation raw material through the action of the upper floating ball, the hydrogenation raw material can simultaneously react inside and outside during the hydrogenation reaction, the reaction efficiency of the hydrogenation reaction is remarkably improved, the condition that the reaction of the hydrogenation raw material on the inner side is easy to be incomplete is effectively avoided, the amount of unsaturated olefin is remarkably reduced, the softening point of the hydrogenation raw material is effectively reduced, and.
The above; but are merely preferred embodiments of the invention; the scope of the invention is not limited thereto; any person skilled in the art is within the technical scope of the present disclosure; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.
Claims (10)
1. A preparation process of petroleum resin with high reaction rate and low softening point is characterized in that: the method comprises the following steps:
s1, distilling a product obtained after the thermal polymerization reaction to obtain molten basic petroleum resin;
s2, mixing and diluting the basic petroleum resin with a hydrogenation solvent, and uniformly stirring to obtain a hydrogenation raw material;
s3, introducing the hydrogenation raw material into a transfer case for hydrogen-containing pretreatment, and then conveying the product subjected to hydrogen-containing pretreatment to a hydrogenation reactor containing a nickel catalyst for hydrogenation reaction;
and S4, removing the hydrogenation solvent after the hydrogenation reaction is finished, and obtaining the petroleum resin with low softening point.
2. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 1, wherein: the mixing volume ratio of the basic petroleum resin to the hydrogenation solvent in the S2 is 1: 2-5.
3. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 1, wherein: the hydrogen-containing pretreatment comprises the following specific operations:
s31, firstly, introducing the hydrogenation raw material into a transfer box;
s32, controlling a sealing pressure plate in the transfer box to move towards the liquid level of the hydrogenation raw material, then introducing inert gas into the transfer box through a gas inlet (22) on the sealing pressure plate, wherein the inert gas permeates into the hydrogenation raw material to form a large amount of bubbles inside the transfer box, and reducing the density of the hydrogenation raw material;
s331, opening the gas inlet (22), overflowing part of the inert gas, then filling hydrogen into the interior through the gas inlet (22), and permeating part of the hydrogen into the low-density hydrogenation raw material;
s332, the upper floating ball in the transfer box is heated under the action of the high-temperature hydrogenation raw material, and the hydrogen in the transfer box overflows and permeates into the hydrogenation raw material from the inner side.
4. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 1, wherein: the total amount of the hydrogen filled in the S331 and the hydrogen in the floating ball is larger than the total amount of the hydrogen needed by the hydrogenation reaction, and the exceeding amount is not larger than 1/5 of the total amount of the needed hydrogen.
5. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 1, wherein: the transfer box comprises a box body (1), a discharge hole (21) is fixedly connected to the right lower end of the box body (1), a sealing pressing plate (3) with an air inlet (22) is in interference fit with the inner wall of the box body (1), and the upper floating ball is fixedly connected to the inner bottom end of the box body (1).
6. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 5, wherein: the sealing pressure plate (3) is positioned at the position of 3-4cm of the upper surface of the hydrogenation raw material.
7. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 5, wherein: the heights of the upper floating balls are different and are uniformly dispersed in the box body (1), and the highest upper floating ball is positioned 5-10cm below the upper surface of the hydrogenation raw material.
8. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 5, wherein: the upper floating ball comprises a flexible pull rope (4) fixedly connected with the inner bottom end of the box body (1) and an air floating ball (5) fixedly connected to the flexible pull rope (4), and hydrogen in a compressed state is filled in the air floating ball (5).
9. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 8, wherein: the air floating ball (5) comprises an upper shaping end (51), a lower air outlet end (52) fixedly connected to the lower end (53) of the upper shaping end (51) and the upper end of the upper shaping end (51), the upper end of the flexible pull rope (4) fixedly penetrates through the middle of the upper shaping end (53) and is fixedly connected with the lower air outlet end (52), hydrogen is located in a space surrounded by the upper shaping end (51) and the upper shaping end (53), and a plurality of uniformly distributed pre-breaking thin sheets (6) are embedded in the upper shaping end (53).
10. The process for preparing petroleum resin with high reaction rate and low softening point as claimed in claim 9, wherein: the upper shaping end (51) is made of a hard material, the upper shaping end (53) and the pre-breaking sheet (6) are made of an elastic material, and the thickness of the pre-breaking sheet (6) is not higher than half of that of the upper shaping end (53).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110079236.9A CN112940155A (en) | 2021-01-21 | 2021-01-21 | Preparation process of petroleum resin with high reaction rate and low softening point |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110079236.9A CN112940155A (en) | 2021-01-21 | 2021-01-21 | Preparation process of petroleum resin with high reaction rate and low softening point |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114106221A (en) * | 2021-12-13 | 2022-03-01 | 马芳 | Preparation method of hydrogenated petroleum resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102453125A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Hydrogenation reaction method of polymer containing olefin unsaturated bonds |
| CN111187383A (en) * | 2020-02-19 | 2020-05-22 | 濮阳市瑞森石油树脂有限公司 | A kind of preparation method of hydrogenated low softening point petroleum resin |
| CN112058185A (en) * | 2020-08-18 | 2020-12-11 | 南京延长反应技术研究院有限公司 | Reaction system and method for petroleum resin hydrogenation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102453125A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Hydrogenation reaction method of polymer containing olefin unsaturated bonds |
| CN111187383A (en) * | 2020-02-19 | 2020-05-22 | 濮阳市瑞森石油树脂有限公司 | A kind of preparation method of hydrogenated low softening point petroleum resin |
| CN112058185A (en) * | 2020-08-18 | 2020-12-11 | 南京延长反应技术研究院有限公司 | Reaction system and method for petroleum resin hydrogenation |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114106221A (en) * | 2021-12-13 | 2022-03-01 | 马芳 | Preparation method of hydrogenated petroleum resin |
| CN114106221B (en) * | 2021-12-13 | 2024-05-10 | 黄骅市丁氏化工新材料有限公司 | Preparation method of hydrogenated petroleum resin |
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