Hydrogenation method of high-chlorine C9 petroleum resin

A petroleum resin and resin technology, applied in the field of hydrogenation of high-chlorine C9 petroleum resin, can solve the problems of complicated process, increased energy consumption, poor removal effect, etc., and achieve the effect of high removal accuracy

Active Publication Date: 2020-08-18
WUHAN KELIN FINE CHEM
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0007] Patent CN105175633A introduces a combined petroleum resin hydrogenation treatment method, which uses alumina and activated carbon to adsorb the resin liquid at high temperature to remove impurities such as sulfur and chlorine in the resin, and then performs two-stage hydrogenation However, in this method, a separator must be installed between the first stage and the second stage hydrogenation reactor, and the resin liquid needs to pass through the separator to separate harmful gases such as hydrogen sulfide and hydrogen chloride in the hydrogenation product before entering the second stage main hydrogenation reactor. Not only the process is cumbersome, but also causes increased energy consumption
[0008] To sum up, at present, for the hydrogenation of high-chlorinated C9 petroleum resin, nickel-molybdenum, cobalt-molybdenum and other sulfurized catalysts can be used for hydrogenation of one-stage hydrogenation, which has strong resistance to impurities such as sulfur and chlorine, excellent stability and long service life. , its disadvantage is that it needs to show better catalytic activity at a higher reaction temperature, and it is easy to cause thermal degradation of C9 petroleum resin, which is not conducive to the improvement of product quality
If a nickel-based reduced state catalyst is used for one-stage hydrogenation, the current general method is to pretreat the resin, and use adsorption to remove part of the sulfur and chlorine impurities in the resin, but the removal effect is poor, and then carry out two stages Hydrogenation, the first stage of hydrogenation is used to further remove impurities such as sulfur and chlorine on the basis of pretreatment, but if the chlorine content is too high, it will cause catalyst poisoning and quickly deactivate its desulfurization ability. In addition, after a stage of hydrogenation To obtain the resin liquid, harmful gases such as hydrogen sulfide and hydrogen chloride in the hydrogenation product must be separated by high and low fractions before entering the second-stage main hydrogenation reactor. Not only the process is cumbersome, but also the energy consumption is increased.

Method used

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Embodiment example

[0022] Below in conjunction with accompanying drawing and specific example the present invention will be further described:

[0023] The technological process that the present invention adopts is figure 1 The technological process in, concrete technological process is as follows:

[0024]Dissolve C9 petroleum resin with a solvent in the resin dissolving tank 1, and the petroleum resin accounts for 10-30% by mass, then mix it with hydrogen, enter the first stage hydrogenation reactor 2 after heating, and carry out hydrogenation adsorption dechlorination removal Chlorine in resin, reaction temperature 150-200°C, pressure 8-17MPa, volume space velocity 1-3h -1 , the volume ratio of hydrogen to oil is 50-200, and the catalyst used is NiCu / Al 2 o 3 -SiO 2 -MgO;

[0025] The first-stage hydrogenation product enters the second-stage hydrogenation reactor 3, and undergoes hydrogenation adsorption desulfurization to remove sulfur in the resin. The reaction temperature is 220-300°C...

Embodiment 1

[0029] C9 resin is dissolved in cyclohexane, the mass ratio of the resin is 20%, the first hydrogenation reaction temperature is 150°C, the pressure is 17MPa, and the volume space velocity is 1h -1 , the volume ratio of hydrogen to oil is 50, and the catalyst used is NiCu / Al 2 o 3 -SiO 2 -MgO, Al used 2 o 3 -SiO 2 -MgO carrier, SiO by mass percent 2 The content is 7%, the MgO content is 9%, and the rest is Al 2 o 3 , the content of active components of the catalyst is based on the total mass of the catalyst. The content of NiO in the active components is 11%, and the content of CuO is 20%. -1 , the volume ratio of hydrogen to oil is 300, and the catalyst is NiZn / Al 2 o 3 , based on the total mass of the catalyst, the content of NiO is 25%, the content of ZnO is 20%, and the rest is Al 2 o 3 ; The temperature of the third hydrogenation reaction is 230°C, the pressure is 17MPa, and the volume space velocity is 0.5h -1 , the volume ratio of hydrogen to oil is 400, and...

Embodiment 2

[0031] C9 resin is dissolved in n-heptane, the mass ratio of the resin is 10%, the first hydrogenation reaction temperature is 200°C, the pressure is 8MPa, and the volume space velocity is 3h -1 , the volume ratio of hydrogen to oil is 130, and the catalyst used is NiCu / Al 2 o 3 -SiO 2 -MgO, Al used 2 o 3 -SiO 2 -MgO carrier, SiO by mass percent 2 The content is 10%, the MgO content is 13%, and the rest is Al 2 o 3 , the content of active components of the catalyst is based on the total mass of the catalyst. The content of NiO in the active components is 15%, and the content of CuO is 16%. -1 , the volume ratio of hydrogen to oil is 450, and the catalyst is NiZn / Al 2 o 3 , based on the total mass of the catalyst, the content of NiO is 35%, the content of ZnO is 10%, and the rest is Al 2 o 3 ; The temperature of the third stage hydrogenation reaction is 320°C, the pressure is 8MPa, and the volume space velocity is 1h -1 , the volume ratio of hydrogen to oil is 800, ...

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Abstract

The invention discloses a hydrogenation method of high-chlorine C9 petroleum resin, which comprises the following steps: (1) feeding a dissolved C9 petroleum resin raw material into a dechlorination tower of a first-stage hydrogenation reactor, and carrying out hydrogenation adsorption dechlorination reaction; (2) feeding the first-stage reaction product into a desulfurization tower of a second-stage hydrogenation reactor, and carrying out a hydrogenation adsorption desulfurization reaction; (3) feeding the second-stage reaction product into a third-stage hydrogenation reactor decolorizing tower, and carrying out olefin and aromatic hydrocarbon hydrogenation saturation reaction; and (4) enabling the third-stage reaction product to sequentially pass through a stripping tower, a normal-pressure distillation tower and a reduced-pressure distillation tower to obtain hydrogenated C9 petroleum resin. The method has the characteristics of simple process, low hydrogenated resin chroma and highresin yield.

Description

technical field [0001] The invention belongs to the technical field of hydrogenation of petroleum resins, and relates to a method for hydrogenation of high-chlorine C9 petroleum resins. Background technique [0002] C9 petroleum resin is a light yellow to dark brown functional resin with a relative molecular weight of 200-3000 and a softening point of 80-140°C. It is a glassy thermoplastic solid at room temperature. At present, the main source of preparing C9 petroleum resin is the by-product of petroleum cracking ethylene. Due to the complex composition of cracking raw materials and the relatively backward production process and production technology of petroleum resin, petroleum resin has deep color and poor stability, especially double bonds, benzene rings, etc. And the presence of a small amount of impurities such as S and N affects the color, stability and compatibility with other resins of the resin, which limits its application range. Hydrogenation of resin is one of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F240/00C08F8/04
CPCC08F8/04C08F240/00Y02W30/62
Inventor 张先茂吴阳春王泽赵志杰夏大寒陈凯郑敏王栋斌王瑜王国兴
Owner WUHAN KELIN FINE CHEM
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