CN112048032A - Preparation method of terpene resin - Google Patents
Preparation method of terpene resin Download PDFInfo
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- CN112048032A CN112048032A CN202010933534.5A CN202010933534A CN112048032A CN 112048032 A CN112048032 A CN 112048032A CN 202010933534 A CN202010933534 A CN 202010933534A CN 112048032 A CN112048032 A CN 112048032A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F32/00—Homopolymers and copolymers of cyclic compounds having no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system
- C08F32/08—Homopolymers and copolymers of cyclic compounds having no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system having two condensed rings
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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Abstract
The invention provides a preparation method of terpene resin, which comprises the steps of adding reaction raw materials and a catalyst into a reaction kettle from the upper end of the reaction kettle, and carrying out a first polymerization reaction; wherein the reaction temperature is 25-32 ℃, the reaction pressure is 0.25-0.35 mPa, and the stirring speed of the reaction kettle is 120-135 r/min; introducing a catalyst by adopting automatic equipment, and adding the catalyst into the reaction kettle at the frequency of 30-60 times per hour; the feeding amount of the reaction kettle is controlled to be 2.5-3M 3/h; and then leading out the obtained product from the middle part of the reaction kettle, circularly mixing and cooling the product by a pump, leading out the part of the product from an outlet of the pump to a next-stage reaction kettle after mixing and cooling, carrying out reaction again, and finally leading out the obtained product to finish the preparation of the terpene resin. Compared with the existing preparation method, the method greatly reduces the generation of organic polymer gel in the preparation process and improves the product quality.
Description
Technical Field
The invention relates to the technical field of terpene resin preparation, in particular to a preparation method of terpene resin.
Background
The terpene resin is processed from turpentine oil, and has the good properties of transparency, no toxicity, neutrality, electric insulativity, hydrophobicity, no crystallization, dilute acid and alkali resistance, heat resistance, light resistance, aging resistance, strong bonding force and the like. The product is widely applied to the aspects of adhesives, double-sided tapes, solvent-based glues, book binding plates, color packages, rubberized fabrics, olefin rubberized fabrics, kraft paper card rubberized fabrics, tape labels, woodworking adhesives, pressure-sensitive adhesives, thermosol, sealants, paints, printing inks and other polymer modifiers and the like.
In the current terpene resin preparation process, turpentine is generally used as a raw material, aluminum trichloride is used as a reaction catalyst, and toluene is used as a solvent to prepare the terpene resin. However, in the actual production process, the preparation of terpene resin still has many problems affecting the quality thereof:
1) the addition of the reaction catalyst is usually that workers directly and manually pour the catalyst into a reaction kettle, and the addition amount of the catalyst is difficult to control, so that the polymerization reaction of turpentine is easy to generate the phenomenon of implosion, the formation of organic polymer gel which is insoluble in toluene is aggravated, and the product quality of terpene resin is seriously influenced; on the other hand, aluminum trichloride is often accompanied with the generation of aluminum hydroxide in the reaction, and when the impurity removal of the product is not complete, in the subsequent process, the aluminum hydroxide can generate coke in a molten state, and the coke can exist in the product in a black spot form, so that the quality of the product is further influenced;
2) the reaction temperature is difficult to control stably, and the condition of rapid rise often occurs, so that the polymerization reaction is extremely unstable, and the gel which is formed by implosion to generate organic macromolecules and is insoluble in toluene is generated, thereby affecting the product quality;
3) the reaction kettle adopted in the prior preparation is usually in a mode of high inlet and low outlet, a discharge hole is usually blocked due to catalyst deposition after long-time use, and the subsequent reaction of the catalyst and raw materials can be influenced.
In view of the above, it is necessary to provide a technical solution to the above problems.
Disclosure of Invention
The invention aims to: provides a preparation method of terpene resin, which can reduce the organic polymer gel which is easily generated in the current terpene resin preparation process to the maximum extent, and control the reaction temperature in a stable range to improve the quality of the final product.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of terpene resin comprises the following steps:
s1, adding reaction raw materials and a catalyst into the reaction kettle from the upper end of the reaction kettle, and carrying out a first polymerization reaction; wherein the reaction temperature is 25-32 ℃, the reaction pressure is 0.25-0.35 mPa, and the stirring speed of the reaction kettle is 120-135 r/min; introducing the catalyst into the reaction kettle by adopting automatic equipment at a frequency of 30-60 times per hour;
s2, after the first polymerization reaction is finished, leading out the obtained product from the middle part of the reaction kettle, mixing and cooling the product, and after mixing and cooling, leading the product into the reaction kettle again from the lower end of the reaction kettle to carry out a second polymerization reaction;
s3, after the second polymerization reaction is finished, leading out the obtained product to finish the preparation of the terpene resin;
wherein the feeding amount of the reaction kettle is controlled to be 2.5-3M 3/h.
Preferably, the moisture content of the reaction raw materials and the catalyst entering the reaction kettle is less than or equal to 150 ppm.
Preferably, the adding amount of the catalyst is 2.4-1.2 kg each time.
Preferably, after the second polymerization reaction is completed and the obtained product is taken out, washing with water, repeating salt filtration and filtration at least twice, distilling and granulating to complete the preparation of the terpene resin.
Preferably, the reaction kettle comprises a kettle body; a motor and a magnetic stirring speed reducer are mounted at the upper end of the kettle body, and the magnetic stirring speed reducer is electrically connected with the motor; a stirring rod electrically connected with the motor is arranged in the kettle body, the two sides of the upper end of the stirring rod are provided with hinge type stirring blades, and the two sides of the lower end of the stirring rod are provided with push type stirring blades; at least three baffles are uniformly arranged on the inner wall of the kettle body; the lower extreme of the cauldron body is provided with the charge door, the middle part of cauldron external side wall is provided with the bin outlet.
Preferably, the hinge type stirring blade is a six-leaf hinge type stirring blade; the push type stirring blade is a six-blade push type stirring blade.
Preferably, the bottom wall of the kettle body is further connected with a material pumping pipeline for pumping out materials in the reaction kettle.
Preferably, the automated equipment employed for introducing the catalyst comprises:
a first sealed reservoir for storing a catalyst;
the weighing device is connected with the first sealed storage and is used for weighing the mass of the catalyst in the first sealed storage;
the three-way valve is connected with the first sealed storage and is used for receiving the catalyst discharged by the first sealed storage;
the reaction kettle is connected with the three-way valve;
and the first gas tank is arranged between the three-way valve and the reaction kettle and is used for blowing the catalyst in the three-way valve into the reaction kettle.
Preferably, a second gas tank and a third gas tank are further arranged between the three-way valve and the reaction kettle, and the blowing direction of the second gas tank and the blowing direction of the third gas tank are different from the blowing direction of the first gas tank, so that the second gas tank and the third gas tank are both used for preventing the catalyst from being blocked.
Preferably, the catalyst introducing system further comprises a recoverer connected to the first sealed storage through a vacuum pipeline and used for receiving excess catalyst discharged in the process of adding the catalyst into the first sealed storage by the second sealed storage.
The invention has the beneficial effects that:
1) according to the preparation method provided by the invention, the preparation method of the terpene resin is improved in aspects of reaction temperature, reaction pressure, stirring speed and feeding amount of a reaction kettle, the times of adding the catalyst per hour and the like, and various reaction conditions are mutually influenced and mutually promoted, so that the quality of the terpene resin product prepared by the method is high, the generation of organic polymer gel in the preparation process is greatly reduced, and the condition that the product quality is further influenced due to the fact that coking substances are generated in the product in the subsequent purification process because of the catalyst and exist in the form of black spots is further reduced.
2) The polymerization reaction is circulated by adopting a middle-outlet and lower-inlet discharging mode, and compared with the traditional top-inlet and bottom-outlet discharging mode, on one hand, the polymerization reaction is more easily matched with the stirring of a reaction kettle for use, so that the homogeneous mixing of reaction materials in the reaction kettle is promoted, the materials are reacted in a homogeneous way, the reaction temperature is further stabilized, and the situation that the temperature is rapidly increased due to the uneven reaction heat release caused by uneven mixing is avoided, the integral polymerization reaction is influenced again, and the domino effect is caused; on the other hand, the condition of catalyst deposition caused by a high-inlet low-outlet feeding mode is avoided, the maintenance frequency of the reaction circulating pump is reduced, the service life of the pump is prolonged, and the production cost is further reduced.
3) The catalyst feeding method provided by the invention is changed into an automatic feeding mode to regulate the adding amount of the catalyst each time and the adding times per hour, so that various problems caused by uncontrollable adding amount due to manual adding are solved. Compared with the traditional catalyst adding mode, the method can adjust the adding amount and frequency of the catalyst at will, accelerate the adding frequency of the catalyst in actual production, reduce the adding amount of each time, ensure that the catalyst and reaction raw materials can be mixed more uniformly, stabilize the reaction temperature in one step, realize the controllability of the reaction temperature and reduce the treatment capacity of washing sewage.
4) In addition, the reaction pressure and the stirring speed are adjusted, the reaction pressure is maintained to be 0.25-0.35 mPa, the stirring speed is increased to 120-135 r/min, and the polymerization reaction of reaction materials is improved to a greater extent by matching with the reaction temperature of 25-30 ℃, so that the generation of organic polymer gel is reduced, and the quality of a final product is improved.
Drawings
FIG. 1 is a schematic structural view of a reaction vessel according to the present invention.
FIG. 2 is a schematic view showing the overall structure of the apparatus of the present invention.
In the figure: 1-a reaction kettle; 11-kettle body; 111-a feed port; 112-a discharge outlet; 113-a material pumping pipeline; 12-a motor; 13-magnetic stirring speed reducer; 14-a stirring rod; 15-a hinge type stirring blade; 16-a propeller type stirring blade; 17-a baffle; 18-an arc-shaped rod; 2-a first recirculating cooling mixer; 3-a second recirculating cooling mixer; 4-a first sealed reservoir; 5-a second sealed reservoir; 6-weighing device; 7-a three-way valve; 81-a first gas tank; 811-pressure regulating valve; 82-a second gas tank; 83-third gas tank; 84-a fourth tank; 9-a recoverer; 91-vacuum pump; 92-a filter screen.
Detailed Description
In order to make the technical solutions and advantages of the present invention clearer, the present invention and its advantages will be described in further detail below with reference to the following detailed description and the accompanying drawings, but the embodiments of the present invention are not limited thereto.
In the description of the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The standard parts used in the invention can be purchased from the market, the special-shaped parts can be customized according to the description of the specification and the accompanying drawings, the specific connection mode of each part adopts conventional means such as bolts, rivets, welding and the like mature in the prior art, the machines, the parts and equipment adopt conventional models in the prior art, and the circuit connection adopts the conventional connection mode in the prior art, so that the detailed description is omitted.
As shown in fig. 1-2, a method for preparing a terpene resin comprises the following steps:
s1, adding reaction raw materials and a catalyst into the reaction kettle 1 from the upper end of the reaction kettle 1 respectively, and carrying out a first polymerization reaction; wherein the reaction temperature is 25-32 ℃, the reaction pressure is 0.25-0.35 mPa, and the stirring speed of the reaction kettle 1 is 120-135 r/min; introducing a catalyst by adopting automatic equipment, and adding the catalyst into the reaction kettle 1 at the frequency of 30-60 times per hour; preferably, the stirring speed of the reaction kettle 1 is 130r/min, compared with the conventional 82r/min rotating speed, the stirring device improves the reaction kettle 1, improves the rotating speed, is more suitable for stirring reaction materials, increases the contact surface between reaction raw materials and a catalyst, further improves the reaction speed, and reduces organic polymer gel generated by implosion;
s2, after the first polymerization reaction is finished, leading out the obtained product from the middle part of the reaction kettle 1, carrying out circular mixing and cooling, and after mixing and cooling, leading the product into the reaction kettle 1 again from the lower end of the reaction kettle 1 to carry out a second polymerization reaction; the product can be reintroduced into the reaction vessel 1 from the bottom wall of the reaction vessel 1; in addition, after the product is circularly mixed and cooled by the pump, part of the product after mixing and cooling can be led out from the outlet of the pump to be partially reacted in a lower-stage reaction kettle;
s3, after the second polymerization reaction is finished, leading out the obtained product to finish the preparation of the terpene resin;
wherein the feeding amount of the reaction kettle 1 is controlled to be 2.5-3M 3/h.
Further, the moisture content of the reaction raw material and the catalyst fed into the reaction tank 1 is 150ppm or less. The low-moisture material can ensure the stability of the catalyst in the reaction process, and prevent aluminum trichloride from hydrolyzing to generate aluminum hydroxide, and supposing that when the generation amount of the aluminum hydroxide is increased, flocculent aluminum hydroxide is mixed with the product and is difficult to strip out, in the subsequent process, the aluminum hydroxide is converted into black coke under the high-temperature state and is accompanied with the generation of irritant gas, so that the quality of the product is influenced, and the physical and psychological health of workers is influenced, therefore, the moisture content of the reaction material is ensured to be less than or equal to 150ppm, the generation of the aluminum hydroxide is favorably reduced, and the stability of the aluminum trichloride catalyst is ensured.
Furthermore, the adding amount of the catalyst is 2.4-1.2 kg each time. In accordance with the above reaction conditions, when the number of times of addition of the catalyst per hour is increased, the amount of the catalyst to be added per hour can be reduced, and the catalyst can be ensured to be sufficiently contacted with the reaction raw material to promote the reaction. The addition of 7kg is reduced by 5.6-6.8 kg on the original basis, the catalyst consumption is reduced to 3% from 5% of the original unit consumption, and if an enterprise calculates according to 9500 ton yield, the aluminum trichloride can be saved by about 200 tons/year, and the workload of sewage treatment is greatly reduced. Preferably, each addition of the catalyst is a uniform addition, preventing gel formation.
Further, after the second polymerization reaction is completed and the obtained product is extracted, washing with water, repeating salt filtration and filtration at least twice, distilling and granulating to complete the preparation of the terpene resin. The repeated salt filtration and filtration are washing which is carried out by salt filtration and filtration at first and then repeated salt filtration and filtration, and the purity of the product can be further ensured after the multiple washing. However, if the salt filtration and filtration steps are reduced, the product cannot be effectively purified after being washed for many times because the washing water is generally recycled water due to simple washing, and the product is generally difficult to stand for a long time to precipitate impurities due to the preparation time after washing. Therefore, the salt filtering and filtering processes are added, so that the cleanliness of the product can be further ensured, and the generation of subsequent coked materials and irritant gases is also avoided.
Further, the reaction kettle 1 adopted by the preparation method comprises a kettle body 11; the upper end of the kettle body 11 is provided with a motor 12 and a magnetic stirring speed reducer 13, and the magnetic stirring speed reducer 13 is electrically connected with the motor 12; a stirring rod 14 electrically connected with the motor 12 is arranged in the kettle body 11, two sides of the upper end of the stirring rod 14 are provided with a hinge type stirring blade 15, and two sides of the lower end of the stirring rod 14 are provided with a push type stirring blade 16; at least three baffles 17 are uniformly arranged on the inner wall of the kettle body 11; the lower extreme of the cauldron body 11 is provided with charge door 111, and the middle part of the external side wall of the cauldron body 11 is provided with bin outlet 112.
This reation kettle 1 has adopted magnetic stirring speed reducer 13 to replace traditional cycloid pinwheel speed reducer, magnetic line of force drives the rotation of the interior magnet steel body of reation kettle 1 in order to drive the rotation of stirring leaf, wherein, hinge formula stirring leaf 15 sets up the upper end at puddler 14, push down and dial to both sides the reaction material stirring during the stirring, and the lower extreme adopts impulse type stirring leaf 16 design, give ascending thrust of reaction material, still set up a plurality of baffles 17 on reation kettle 1's the inner wall simultaneously, for reaction material improves a counter force, avoided reaction material to stir along same direction always, two kinds of stirring leaves and baffle 17 combined action, the abundant contact of reaction raw materials and catalyst has been strengthened greatly, promote polymerization's going on, and improve production efficiency, reduce the implosion phenomenon that appears in the polymerization simultaneously, reduce the formation of organic polymer gel.
Preferably, the hinge type stirring blade 15 is a six-blade hinge type stirring blade; the push type stirring blade 16 is a six-blade push type stirring blade. Of course, the flap-type stirring vanes 15 may be designed as four-leaf flap-type stirring vanes, five-leaf flap-type stirring vanes, or the like, depending on the size of the reaction vessel 1, the amount of the reaction raw material, and the like. And the impeller 16 may be a six-blade impeller. The push type stirring blades 16 are arranged corresponding to the hinge type stirring blades 15 and are uniformly distributed on two sides of the stirring rod 14. Preferably, the inclination angle of the blades of the hinged stirring blades 15 can be 30 °, 45 ° or 60 °, and the vortex formed by the inclination angles can more easily promote the mixing of the reaction materials. Specifically, in the reaction vessel 1 having a volume of 8000L, the diameter of the stirring vanes was 800mm, and the size of the baffle 17 was 1000 × 200 × 20 mm. Wherein, the baffle 17 position in fig. 1 is the schematic diagram, and in the actual reation kettle, the baffle 17 is evenly set up on the inner wall of cauldron body 1, avoids the position of discharge gate 12 to set up.
Further, the blade length of the flap-type stirring vanes 15 is smaller than the blade length of the pusher-type stirring vanes 16. The length of the blade of the stirring blade at the lower end is longer than that of the blade at the upper end, so that the reaction materials can be received more conveniently, most of the reaction raw materials are always kept to move back and forth among the folding stirring blade 15, the push stirring blade 16 and the baffle 17, the contact between the reaction raw materials and the catalyst is promoted to a greater extent, the more uniform the reaction materials are mixed, the faster the reaction system is, and the aim of improving the reaction efficiency on the whole is fulfilled.
Further, the bottom wall of the kettle body 11 is connected with a material pumping pipeline 113 for pumping out materials in the reaction kettle 1. The kettle body 11 is additionally provided with a material extracting pipeline 113 for extracting reactants in the kettle body 11 so as to be convenient for maintenance and detection of the kettle body 11.
Further, the reaction kettle 1 is also sequentially connected with the first circulating cooling mixer 2 and the second circulating cooling mixer 3, and is used for mixing and cooling the materials led out from the reaction kettle 1, so that one circulation of material reaction is realized. In the actual production, the solvent is added into the reaction vessel 1 in advance, and then other reaction materials are added, in the whole cycle of the polymerization reaction, a certain amount of reaction materials are reserved in the reaction vessel 1, that is, the product extracted in step S2 is a partial product, so as to realize the whole cycle of the reaction in the reaction vessel 1.
Further, the automatic equipment adopted by the preparation method for introducing the catalyst comprises: comprises a first sealed storage 4 for storing catalyst, a weighing device 6, a three-way valve 7, a first gas tank 81 and a reaction kettle 1; wherein, the weighing device 6 is connected with the first sealed storage 4 and is used for weighing the mass of the catalyst in the first sealed storage 4; the three-way valve 7 is connected with the first sealed storage 4 and is used for receiving the catalyst discharged from the first sealed storage 4; the reaction kettle 1 is connected with a three-way valve 7; and a first gas tank 81 arranged between the three-way valve 7 and the reaction kettle 1 and used for blowing the catalyst in the three-way valve 7 into the reaction kettle 1. The catalyst is a liquid doped with 5% solid aluminum trichloride, the viscosity is 80-100 cps, and the average specific gravity is 0.93. The scale 6 may be an electronic pound.
Further, a second air tank 82 and a third air tank 83 are provided between the three-way valve 7 and the reaction kettle 1, and the blowing directions of the second air tank 82 and the third air tank 83 are different from the blowing direction of the first air tank 81, so as to prevent the catalyst from being blocked. Specifically, the blow-up direction of the second gas tank 82 is opposite to the blow-up direction of the first gas tank 81; the blow-up direction of the third gas tank 83 is set at 90 degrees to the blow-up direction of the first gas tank 81; the third gas tank 83 and the first gas tank 81 may be provided at one end of the reaction vessel 1, and the second gas tank 82 may be provided at the other end of the reaction vessel 1, and the third gas tank 83 may assist the first gas tank 81 in blowing the catalyst into the reaction vessel 1, while also functioning as a blockage prevention.
Further, the catalyst introducing system further comprises a second sealed reservoir 5 connected to the first sealed reservoir 4 for adding the catalyst to the first sealed reservoir 4. The second sealed storage 5 can be a catalyst storage bag, and the catalyst in the second sealed storage is added into the first sealed storage 4, so that the catalyst can be automatically introduced into the reaction kettle 1.
Further, the catalyst introducing system also comprises a recoverer 9 which is connected with the first sealed storage 4 through a vacuum pipeline and is used for receiving the redundant catalyst discharged in the process that the second sealed storage 5 adds the catalyst into the first sealed storage 4. When the second sealed storage 5 adds the catalyst into the first sealed storage 4, the vacuum pump 91 connected with the upper end of the recoverer 9 is started at the same time, a certain vacuum is charged into the first sealed storage 4, then the vacuum valve in the vacuum pump 91 introduces the catalyst in the second sealed storage 5 into the first sealed storage 4, and the catalyst led out along with the vacuum pipeline or redundant catalyst is introduced into the recoverer 9 through the vacuum pipeline, so that the catalyst is prevented from scattering into the external environment, the waste of the catalyst is avoided, and the physical and mental health of workers is influenced. After the first hermetic container 4 finishes the catalyst suction, the vacuum pump 91 is turned off, and then the catalyst in the first hermetic container 4 is blown into the reaction tank 1.
Further, a filter screen 92 is provided at the upper part of the recovery unit 9. The arrangement of the filter screen 92 prevents the introduced catalyst from gathering in a large amount at the upper part of the recoverer 9 and attaching to the upper part of the recoverer 9, which not only affects the cleaning of the recoverer 9, but also causes the waste of the catalyst. The screen 92 may be an 80 mesh nylon screen.
Further, a fourth gas tank 84 is connected to the upper end of the recovery unit 9, and the fourth gas tank 84 is used for blowing the catalyst in the upper part of the recovery unit 9 to the lower part.
Further, the lower end of the recoverer 9 is connected with the reaction kettle 1. The catalyst in the recoverer 9 can also be directly introduced into the reaction kettle 1, so that the utilization rate of the catalyst is improved.
Further, the gas carried in the first gas tank 81, the second gas tank 82, the third gas tank 83, and the fourth gas tank 84 is nitrogen gas. In addition, the upper part of the first sealed reservoir 4 can be filled with a part of nitrogen gas to protect the stability of the catalyst in the reservoir.
Further, the first gas tank 81 is provided with a pressure regulating valve 811, and the pressure regulating valve 811 regulates pressure of 0.20 to 0.4 mPa. The nitrogen blowing rate and frequency are controlled by the pressure control valve 811, and the amount of catalyst entering the reactor 1 each time is controlled. In the actual production, the blowing frequency of the catalyst per hour can be improved, the blowing amount of the catalyst per hour can be reduced, the contact area between the catalyst in the reaction kettle 1 and the reaction raw materials and the mixing uniformity can be further realized, and the reaction efficiency and the product yield can be improved.
In addition, in combination with an automatic device for introducing a catalyst, the reaction kettle 1 is connected with the second sealed storage 5, and the reaction kettle 1 further comprises a temperature detector for detecting the reaction temperature in the reaction kettle 1. The change of the reaction temperature is obtained by detecting the reaction temperature, and the aging time is further utilized to judge the requirement condition of the catalyst. And the catalyst introduces the volume that weighing device 6, three-way valve 7 and first gas pitcher 81 that set up in the automation equipment added, and then the addition of adjustment catalyst according to the demand condition of catalyst, not only makes holistic reaction more complete, and the product yield is higher, can reach the rational utilization to reaction materials such as catalyst simultaneously, improves reaction material's utilization ratio, reduction in production cost.
The terpene resin finally produced by the invention not only greatly reduces the impurities such as organic polymer gel and the like which can be doped in the terpene resin, but also effectively improves the molecular structure of the product, improves the production efficiency and the product yield, and reduces the production cost of enterprises from multiple dimensions by improving the preparation process in multiple aspects and realizing the interaction and the mutual influence among the parameter adjustment.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. The preparation method of the terpene resin is characterized by comprising the following steps:
s1, adding reaction raw materials and a catalyst into the reaction kettle from the upper end of the reaction kettle, and carrying out a first polymerization reaction; wherein the reaction temperature is 25-32 ℃, the reaction pressure is 0.25-0.35 mPa, and the stirring speed of the reaction kettle is 120-135 r/min; introducing the catalyst into the reaction kettle by adopting automatic equipment at a frequency of 30-60 times per hour;
s2, after the first polymerization reaction is finished, leading out the obtained product from the middle part of the reaction kettle, mixing and cooling the product, and after mixing and cooling, leading the product into the reaction kettle again from the lower end of the reaction kettle to carry out a second polymerization reaction;
s3, after the second polymerization reaction is finished, leading out the obtained product to finish the preparation of the terpene resin;
wherein the feeding amount of the reaction kettle is controlled to be 2.5-3M 3/h.
2. The method for preparing terpene resin according to claim 1, wherein the moisture content of the reaction raw material and the catalyst entering the reaction vessel is 150ppm or less.
3. The method for preparing terpene resin according to claim 1, wherein the amount of the catalyst added per time is 2.4 to 1.2 kg.
4. The method of claim 1, wherein the second polymerization is performed to extract the product, the product is washed with water, the salt filtration and filtration are repeated at least twice, the distillation and the granulation are performed to complete the terpene resin.
5. The method for preparing terpene resin according to claim 1, wherein the reaction vessel comprises a vessel body; a motor and a magnetic stirring speed reducer are mounted at the upper end of the kettle body, and the magnetic stirring speed reducer is electrically connected with the motor; a stirring rod electrically connected with the motor is arranged in the kettle body, the two sides of the upper end of the stirring rod are provided with hinge type stirring blades, and the two sides of the lower end of the stirring rod are provided with push type stirring blades; at least three baffles are uniformly arranged on the inner wall of the kettle body; the lower extreme of the cauldron body is provided with the charge door, the middle part of cauldron external side wall is provided with the bin outlet.
6. The method for preparing terpene resin according to claim 5, wherein the flap-type stirring blade is a hexalobular flap-type stirring blade; the push type stirring blade is a six-blade push type stirring blade.
7. The method for preparing terpene resin as claimed in claim 5, wherein the bottom wall of the reactor is further connected with a material-pumping pipeline for pumping out the materials in the reactor.
8. The method of claim 1, wherein the automated equipment used to introduce the catalyst comprises:
a first sealed reservoir for storing a catalyst;
the weighing device is connected with the first sealed storage and is used for weighing the mass of the catalyst in the first sealed storage;
the three-way valve is connected with the first sealed storage and is used for receiving the catalyst discharged by the first sealed storage;
the reaction kettle is connected with the three-way valve;
and the first gas tank is arranged between the three-way valve and the reaction kettle and is used for blowing the catalyst in the three-way valve into the reaction kettle.
9. The method for producing terpene resin according to claim 8, wherein a second gas tank and a third gas tank are further provided between the three-way valve and the reaction vessel, and the second gas tank and the third gas tank are blown in different directions from the first gas tank, both for preventing clogging of the catalyst.
10. The method of claim 8, wherein the catalyst introduction system further comprises a recovery device connected to the first sealed reservoir via a vacuum line for receiving excess catalyst discharged during the addition of catalyst from the second sealed reservoir to the first sealed reservoir.
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| CN202010933534.5A CN112048032A (en) | 2020-09-08 | 2020-09-08 | Preparation method of terpene resin |
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| CN202010933534.5A CN112048032A (en) | 2020-09-08 | 2020-09-08 | Preparation method of terpene resin |
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| CN202010933534.5A Pending CN112048032A (en) | 2020-09-08 | 2020-09-08 | Preparation method of terpene resin |
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| CN (1) | CN112048032A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB577384A (en) * | 1943-12-02 | 1946-05-16 | Samuel Gross Burroughs | Terpene resin |
| US2483124A (en) * | 1948-07-06 | 1949-09-27 | Pennsylvania Ind Chemical Corp | Method of making terpene resin |
| CN1631916A (en) * | 2004-11-21 | 2005-06-29 | 蓝运泉 | Production method of terpene resin |
| CN102351991A (en) * | 2011-10-19 | 2012-02-15 | 濮阳市瑞森石油树脂有限公司 | Equipment and method for controlling polymerization temperature of petroleum resin |
| CN102898564A (en) * | 2012-11-01 | 2013-01-30 | 张道飘 | Method for preparing terpene resin |
| CN103288992A (en) * | 2013-05-31 | 2013-09-11 | 罗定市星光化工有限公司 | Method and special device for adding catalyst in polymerization reaction for producing polyterpene resin |
| CN204589046U (en) * | 2015-04-15 | 2015-08-26 | 罗定市星光化工有限公司 | The specific equipment of catalyzer is dripped in the polyreaction that terpine resin is produced |
| CN206027709U (en) * | 2016-08-31 | 2017-03-22 | 濮阳班德路化学有限公司 | Terpene resin's polymerization jar |
| CN109485765A (en) * | 2018-12-07 | 2019-03-19 | 江西瑞源食品科技有限公司 | A kind of new process of terpene resin preparation |
-
2020
- 2020-09-08 CN CN202010933534.5A patent/CN112048032A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB577384A (en) * | 1943-12-02 | 1946-05-16 | Samuel Gross Burroughs | Terpene resin |
| US2483124A (en) * | 1948-07-06 | 1949-09-27 | Pennsylvania Ind Chemical Corp | Method of making terpene resin |
| CN1631916A (en) * | 2004-11-21 | 2005-06-29 | 蓝运泉 | Production method of terpene resin |
| CN102351991A (en) * | 2011-10-19 | 2012-02-15 | 濮阳市瑞森石油树脂有限公司 | Equipment and method for controlling polymerization temperature of petroleum resin |
| CN102898564A (en) * | 2012-11-01 | 2013-01-30 | 张道飘 | Method for preparing terpene resin |
| CN103288992A (en) * | 2013-05-31 | 2013-09-11 | 罗定市星光化工有限公司 | Method and special device for adding catalyst in polymerization reaction for producing polyterpene resin |
| CN204589046U (en) * | 2015-04-15 | 2015-08-26 | 罗定市星光化工有限公司 | The specific equipment of catalyzer is dripped in the polyreaction that terpine resin is produced |
| CN206027709U (en) * | 2016-08-31 | 2017-03-22 | 濮阳班德路化学有限公司 | Terpene resin's polymerization jar |
| CN109485765A (en) * | 2018-12-07 | 2019-03-19 | 江西瑞源食品科技有限公司 | A kind of new process of terpene resin preparation |
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