CN111250022A - Preparation method of BMC (bulk molding compound) molding resin - Google Patents
Preparation method of BMC (bulk molding compound) molding resin Download PDFInfo
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- CN111250022A CN111250022A CN202010164097.5A CN202010164097A CN111250022A CN 111250022 A CN111250022 A CN 111250022A CN 202010164097 A CN202010164097 A CN 202010164097A CN 111250022 A CN111250022 A CN 111250022A
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Abstract
The invention relates to a preparation method of BMC (bulk molding compound) molding resin, which comprises the following steps: feeding materials according to the feeding sequence; after the feeding is finished, adding corresponding auxiliary agents and small materials, and slowly opening a heating oil valve to start heating; the first step is that the material is heated to water, then the temperature is slowly raised from the water temperature, nitrogen is introduced in the heating process, then the sampling is carried out to measure the acid value, and the cooling is carried out; after the material temperature is cooled, feeding a second step material and an auxiliary agent; secondly, heating up the materials after feeding, discharging water, performing heat preservation reaction after discharging water, heating up and preserving heat, introducing nitrogen in the heating process, preserving heat and measuring the acid value; when the acid value reaches the standard, the viscosity of a vertebral plate of polyester at 150 ℃ reaches the standard, the vacuum is started, after the viscosity is qualified, the vertebral plate is cooled, JQ and PQ hydroquinone are added, the material temperature is continuously cooled, and dilution is carried out; adding small materials DQ and T50 before diluting; compared with the prior art, the method improves the quality stability of the BMC die pressing resin and improves the strength and hardness of the BMC die pressing resin.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a preparation method of BMC (bulk molding compound) molding resin.
Background
Unsaturated Polyester Resin (UPR) is a linear high molecular compound with multifunctional groups, a backbone of the unsaturated polyester resin has polyester chain bonds and unsaturated double bonds, and both ends of a macromolecular chain respectively have carboxyl and hydroxyl, the most important advantage of using the unsaturated polyester resin is that a diluent of the unsaturated polyester resin generates copolymerization crosslinking reaction with the double bonds on the backbone when in final use, so the volatilization amount of a solvent in the use process is less, the unsaturated polyester resin belongs to a product with environmental protection, the product is often used as a matrix in the field of SMC/BMC products, a bulk BMC molding compound is also called as unsaturated polyester glass fiber reinforced molding compound, the main raw material of the unsaturated polyester resin is a bulk prepreg which is formed by fully mixing chopped glass fibers, the unsaturated polyester resin, fillers and various additives, and belongs to one of thermosetting molding compound molding materials and is mainly applied to electrical appliances, in the fields of motors, automobiles, buildings, daily goods and the like, block-shaped molding materials are continuously developed and improved for decades, but the batch quality of products is still unstable, and the tensile strength, bending strength and bus hardness are not high, so that improvement is necessary.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of BMC (bulk molding compound) molding resin with stable batch quality and high strength and hardness.
The technical scheme of the invention is realized as follows: a preparation method of BMC molding resin is characterized in that: the method comprises the following steps:
s1: before feeding, nitrogen is introduced into the esterification reaction kettle, and the states of valves, a water outlet system and valves of a vacuum buffer tank are checked.
S2: checking the name and the quantity of the raw materials, and sequentially feeding the raw materials according to a feeding sequence after the raw materials are accurately confirmed; firstly, liquid alcohol is added, after the alcohol is added, the mixture is preheated to 80-90 ℃, and then solid materials (neopentyl glycol, phthalic anhydride and triphenyl ester are added in sequence) are added.
S3: after the feeding is finished, adding corresponding auxiliary agents and small materials, slowly opening a heating (large and small) oil valve to start heating, observing the reaction condition of the materials in the reaction kettle, taking emergency measures in time when an abnormal condition is found, and reporting to a production department.
S4: the first step is that the material is heated to water, and then the temperature of the water is slowly heated to 195 +/-1 ℃, the process needs about 5 hours, the temperature of the top of the tower is controlled not to exceed 103 ℃ in the heating process, nitrogen (3-5 m3/h) is introduced in the heating process to reach the required temperature (195 ℃), and then the sampling acid value is measured to be 30-40 mgKOH/g, so that the material can be cooled.
S5: cooling the material to below 150 deg.C to prepare the second step material and adjuvant (the feeding sequence is propylene glycol, liquid anhydride, triphenyl ester and hydroquinone).
S6: and (2) after the materials are fed, heating to 162 +/-2 ℃ to discharge water, carrying out heat preservation reaction for 0.5 hour after water discharge, heating to 208 +/-1 ℃ to preserve heat, carrying out heat preservation at a constant speed for about 6 hours after water discharge, introducing nitrogen gas for 3-5 m3/h in the heating process, controlling the temperature at the top of the tower to be not more than 103 ℃, preserving heat for about 3 hours, and measuring the acid value.
S7: when the acid value is 62-68 mgKOH/g, the viscosity of the polyester vertebral plate at 150 ℃ is as follows: 1.0-1.4P, starting vacuum, wherein the vacuum time is about 4-4.5 hours (the vacuum degree is more than-0.092 Mpa), the acid value after vacuum is 26-28 mgKOH/g, and the viscosity of a polyester vertebral plate at 150 ℃ is as follows: 10.5 to 11P, cooling to 180 +/-1 ℃ after the product is qualified, adding JQ and PQ hydroquinone, and continuously cooling the material to 158 +/-2 ℃ until the material temperature is reached, so that dilution can be carried out. (the time from the addition of JQ to the start of thinning is not less than 40 minutes)
S8: and before diluting, ensuring that the styrene is injected into the diluting kettle, starting stirring the diluting kettle, adding DQ and T50 small materials in advance, then starting diluting, controlling the diluting flow and the diluting kettle material temperature in the diluting process, controlling the highest material temperature of the diluting kettle at 80-83 ℃ after diluting is finished, and optimally controlling the diluting time at 40-60 minutes.
S9: cooling to about 70 ℃ after the dilution is finished, adding copper naphthenate, dehydrating for 40 minutes in vacuum, continuously cooling to about 65 ℃, sampling, detecting, filtering and packaging after the product is qualified.
By adopting the technical scheme, the temperature, the reaction time and the acid value of the BMC molding resin in the production process are controlled by strict process standards, and the BMC molding resin is prepared after strict production process.
The invention is further configured to: the raw materials comprise 1275kg of phthalic anhydride, 1230kg of propylene glycol and 3kg of triphenyl phosphite of the first step material; 3650kg of maleic anhydride, 1000kg of methyl propylene glycol, 1580kg of propylene glycol, 3kg of triphenyl phosphite and 2200g of hydroquinone in the second step; 3650kg of auxiliary agent and small materials of styrene, JQ2000g, DQ800g, T504000 g, CU260g and 50kg of replenishing concentrated solution.
By adopting the technical scheme, the BMC molding resin is prepared by mixing 1275kg of phthalic anhydride, 1230kg of propylene glycol, 6kg of triphenyl phosphite, 3650kg of maleic anhydride, 1000kg of methyl propylene glycol, 1580kg of propylene glycol, 2200g of hydroquinone, 3650kg of styrene, JQ2000g, DQ800g, T504000 g, CU260g and 50kg of thickening fluid, wherein the content of each component is fixed, so that the optimal proportioning and mixing effect is achieved, and the BMC molding resin is prepared by a reaction kettle and a diluting kettle through composite stirring.
The invention also discloses a reaction kettle suitable for the BMC molding resin preparation method, which is characterized in that: the stirring device comprises a kettle body, wherein a feed inlet and a discharge outlet are arranged on the kettle body, a stirring rod is arranged in the kettle body, a stirring motor is arranged on the upper surface of the kettle body, the upper end of the stirring rod is fixedly connected with the output end of the stirring motor, a first stirring assembly is arranged at one end, far away from the stirring motor, of the stirring rod, the first stirring assembly comprises a first stirring ring, a second stirring ring and a third stirring ring which are concentrically arranged and in a circular ring shape, the diameters of the first stirring ring, the second stirring ring and the third stirring ring are sequentially reduced, the upper portion of the first stirring ring is fixedly connected with one end, far away from the stirring motor, of the stirring rod, the outer ring wall of the second stirring ring is provided with two first rotating connecting rods, the two first rotating connecting rods are symmetrically arranged on two sides of the outer ring wall of the second stirring rod by taking the center of the second stirring ring as a symmetry point, two first rotating holes matched with the two first rotating connecting rods are arranged on the inner ring wall of the first stirring, an included angle between a connecting line between the two first rotating holes and a horizontal plane is 45 degrees or 135 degrees, a first bearing is arranged in each first rotating hole, the first rotating connecting rods are rotatably connected in the first rotating holes through the first bearings, two second rotating connecting rods are arranged on the outer ring wall of the third stirring ring, the two second rotating connecting rods are symmetrically arranged on two sides of the outer ring wall of the third stirring rod by taking the ring center of the third stirring ring as a symmetrical point, two second rotating holes matched with the two second rotating connecting rods are arranged on the inner ring wall of the second stirring ring, the included angle between the connecting line between the two second rotating holes and the horizontal plane is 90 degrees different from the connecting line between the two first rotating holes, a second bearing is arranged in each second rotating hole, the second rotating connecting rods are rotatably connected in the second rotating holes through the second bearings, and sealing rings are arranged at the orifices of the first rotating holes and the second rotating holes, one side of the first stirring ring, which is far away from the stirring rod, is fixedly provided with a stirring part, and the lower part of the outer side wall of the kettle body is provided with a sampling assembly.
By adopting the technical scheme, in the process of producing BMC (bulk molding compound) mould pressing resin, the feed inlet on the kettle body is opened, each part of raw material after the inspection is finished is put into the kettle body from the feed inlet of the kettle body in sequence, then the feed inlet is closed, the stirring motor on the upper surface of the kettle body is started, the stirring motor drives the stirring rod to rotate, the rotating stirring rod drives the first stirring assembly and the stirring part to rotate, the first stirring ring rotates coaxially with the stirring rod along with the rotation of the stirring rod, the second stirring ring stirs the raw material in the kettle body at the first stirring ring and the stirring part, the first rotating connecting rod on the second stirring ring is mutually matched with the first bearing in the first rotating hole to enable the second stirring ring to rotate along with the rotation of the first stirring ring and the flowing of the raw material by using the connecting line of the two first rotating holes as a rotating shaft, and the second rotating connecting rod on the third stirring ring is mutually matched with the second bearing in the second rotating hole to enable the third stirring ring to use the two second stirring rings along with the rotation of The connection line of the two rotating holes is a rotating shaft to rotate, raw materials in the kettle body generate different flow directions in the mixing process through the different rotating directions of the first stirring ring, the second stirring ring and the third stirring ring, so that the raw materials are fully mixed, sampling detection is carried out through the sampling assembly after the raw materials are fully mixed, and a discharge port on the kettle body is opened to discharge the raw materials after the raw materials are detected to be qualified.
The present invention is preferably: the sampling assembly comprises a discharging pipe and a collecting bottle, the discharging pipe is fixedly arranged at the lower part of the outer side wall of the kettle body and is communicated with the interior of the kettle body, a valve is arranged in the discharging pipe, a connecting part is arranged at one end of the collecting bottle, a connecting pipeline is arranged in the connecting part and is communicated with the bottle cavity of the collecting bottle, the outer diameter of the connecting part is the same as the inner diameter of the pipeline of the discharging pipe and is matched with the inner diameter of the pipeline of the discharging pipe, a clamping assembly is arranged on the outer side wall of the connecting part and comprises a clamping block, a clamping block mounting cavity and a plurality of springs, the clamping block mounting cavity is arranged on the outer side wall of the connecting part, the vertical cross section of the clamping block mounting cavity is in a concave shape, openings are formed in the outer side wall of the connecting part at two ends of the clamping block, the vertical cross section of the clamping block is in, one end of the spring is fixedly connected with the inner wall of the clamping block mounting cavity on one side of the opening, the other end of the spring is fixedly connected with the outer wall of the clamping block on one side of the opening, the clamping groove matched with the clamping block is formed in one side, away from the kettle body, of the inner wall of the discharge pipe, one end, away from the material collecting bottle, of the connecting portion is provided with a first sealing ring, and a second sealing ring matched with the first sealing ring is fixedly arranged on the inner wall of the pipeline of the discharge pipe.
By adopting the technical scheme, in the process of producing BMC (bulk molding compound) mould pressing resin, after raw materials are fully mixed, the stirring motor is shut down, then one end of the clamping block on the connecting part of the collecting bottle is pressed close to the collecting bottle, one end of the clamping block is pressed into the clamping block mounting cavity, the spring is compressed, the other end of the clamping block is retracted into the clamping block mounting cavity, then the connecting part of the collecting bottle is inserted into the discharging pipe, after the connecting part is inserted into the discharging pipe, the clamping block is loosened, the compressed spring ejects the clamping block out of the clamping block mounting cavity, one end of the clamping block is positioned outside the discharging pipe and in the discharging pipe, one end of the clamping block in the discharging pipe is matched with the clamping groove after being ejected by the spring to fix the connecting part in the discharging pipe, after the connecting part is fixed, the first sealing ring is abutted to the second sealing ring, then the valve, the material collecting bottle is convenient to sample, the phenomenon that a large amount of air enters the kettle body in the sampling process is reduced, the phenomenon that the kettle body is scalded by the high temperature of the raw materials in the sampling process is reduced, and the sampling efficiency is improved.
The present invention is preferably: the bottleneck of the collecting bottle is conical.
By adopting the technical scheme, the tapered bottle mouth can reduce the raw material residue in the collecting bottle when the raw material is poured out from the collecting bottle.
The present invention is preferably: and an electric heating device is fixedly arranged at the bottom of the material collecting bottle.
Through adopting above-mentioned technical scheme, electric heating device can prevent that the aggregate bottle temperature from crossing lowly to lead to the raw materials to solidify and influence and get the material and detect, makes the raw materials keep liquid state and has also reduced the remaining phenomenon of raw materials in the aggregate bottle simultaneously.
The present invention is preferably: and a pressure release valve is arranged on the outer side wall of the kettle body.
Through adopting above-mentioned technical scheme, at the in-process of production BMC mould pressing resin, the pressure relief valve on the lateral wall of the cauldron body can in time open the internal pressure of the cauldron of letting out when internal pressure of cauldron is too big, reduces to appear because of the too big phenomenon that leads to the cauldron body explosion of pressure, has improved the security of the cauldron body.
The invention also discloses an operation method of the reaction kettle suitable for BMC molding resin, which is characterized by comprising the following steps: the method comprises the following steps:
firstly, feeding raw materials: and opening a feed inlet on the kettle body, sequentially putting all the checked raw materials into the kettle body from the feed inlet of the kettle body, and then closing the feed inlet.
Secondly, stirring and mixing the raw materials: the agitator motor of start-up cauldron body upper surface, agitator motor drive the puddler and rotate, and the pivoted puddler drives first stirring subassembly and stirring portion and rotates, and first stirring subassembly rotates and stirs the raw materials in the cauldron body with stirring portion, makes the raw materials intensive mixing.
Thirdly, sampling and detecting: after the raw materials intensive mixing, turn off agitator motor, then insert the connecting portion of collecting bottle discharging pipe, make joint subassembly on the connecting portion mutually support with draw-in groove on the discharging pipe pipeline inner wall, and make first sealing washer and second sealing washer butt, then open the valve on the discharging pipe, close the valve after filling with the raw materials in waiting the collecting bottle, take down the collecting bottle on by the discharging pipe, and wash the discharging pipe with the clear water, detect in the collecting bottle at last.
Fourthly, discharging raw materials: and after the raw materials are detected to be qualified, opening a discharge hole on the kettle body to discharge the raw materials from the kettle body.
Fifthly, cleaning the kettle body: after the raw materials are discharged, the interior of the kettle body is washed by clear water and is ready for the next reaction.
By adopting the technical scheme, the mixing sufficiency of the raw materials in the reaction kettle body in the stirring and mixing process is improved, so that the quality stability of the BMC (bulk molding compound) molding resin is improved, and the strength and hardness of the BMC molding resin are improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of the first stirring assembly.
Fig. 3 is a partially enlarged view of a portion a in fig. 1.
Labeled as: 1-kettle body, 2-feeding hole, 3-discharging hole, 4-stirring rod, 5-stirring motor, 6-first stirring ring, 7-second stirring ring, 8-third stirring ring, 9-first rotating connecting rod, 10-first rotating hole, 11-first bearing, 12-sealing ring, 13-stirring part, 14-discharging pipe, 15-material collecting bottle, 16-valve, 17-connecting part, 18-clamping block, 19-clamping block mounting cavity, 20-spring, 21-clamping groove, 22-first sealing ring, 23-second sealing ring, 24-electric heating device and 25-pressure relief valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 to 3, the present invention discloses a method for preparing BMC molding resin, in the specific embodiment of the present invention: the method comprises the following steps:
s1: before feeding, nitrogen is introduced into the esterification reaction kettle, and the states of valves, a water outlet system and valves of a vacuum buffer tank are checked.
S2: checking the name and the quantity of the raw materials, and sequentially feeding the raw materials according to a feeding sequence after the raw materials are accurately confirmed; firstly, liquid alcohol is added, after the alcohol is added, the mixture is preheated to 80-90 ℃, and then solid materials (neopentyl glycol, phthalic anhydride and triphenyl ester are added in sequence) are added.
S3: after the feeding is finished, adding corresponding auxiliary agents and small materials, slowly opening a heating (large and small) oil valve to start heating, observing the reaction condition of the materials in the reaction kettle, taking emergency measures in time when an abnormal condition is found, and reporting to a production department.
S4: the first step is that the material is heated to water, and then the temperature of the water is slowly heated to 195 +/-1 ℃, the process needs about 5 hours, the temperature of the top of the tower is controlled not to exceed 103 ℃ in the heating process, nitrogen (3-5 m3/h) is introduced in the heating process to reach the required temperature (195 ℃), and then the sampling acid value is measured to be 30-40 mgKOH/g, so that the material can be cooled.
S5: cooling the material to below 150 deg.C to prepare the second step material and adjuvant (the feeding sequence is propylene glycol, liquid anhydride, triphenyl ester and hydroquinone).
S6: and (2) after the materials are fed, heating to 162 +/-2 ℃ to discharge water, carrying out heat preservation reaction for 0.5 hour after water discharge, heating to 208 +/-1 ℃ to preserve heat, carrying out heat preservation at a constant speed for about 6 hours after water discharge, introducing nitrogen gas for 3-5 m3/h in the heating process, controlling the temperature at the top of the tower to be not more than 103 ℃, preserving heat for about 3 hours, and measuring the acid value.
S7: when the acid value is 62-68 mgKOH/g, the viscosity of the polyester vertebral plate at 150 ℃ is as follows: 1.0-1.4P, starting vacuum, wherein the vacuum time is about 4-4.5 hours (the vacuum degree is more than-0.092 Mpa), the acid value after vacuum is 26-28 mgKOH/g, and the viscosity of a polyester vertebral plate at 150 ℃ is as follows: 10.5 to 11P, cooling to 180 +/-1 ℃ after the product is qualified, adding JQ and PQ hydroquinone, and continuously cooling the material to 158 +/-2 ℃ until the material temperature is reached, so that dilution can be carried out. (the time from the addition of JQ to the start of thinning is not less than 40 minutes)
S8: and before diluting, ensuring that the styrene is injected into the diluting kettle, starting stirring the diluting kettle, adding DQ and T50 small materials in advance, then starting diluting, controlling the diluting flow and the diluting kettle material temperature in the diluting process, controlling the highest material temperature of the diluting kettle at 80-83 ℃ after diluting is finished, and optimally controlling the diluting time at 40-60 minutes.
S9: cooling to about 70 ℃ after the dilution is finished, adding copper naphthenate, dehydrating for 40 minutes in vacuum, continuously cooling to about 65 ℃, sampling, detecting, filtering and packaging after the product is qualified.
By adopting the technical scheme, the temperature, the reaction time and the acid value of the BMC molding resin in the production process are controlled by strict process standards, and the BMC molding resin is prepared after strict production process.
In a specific embodiment of the invention: the raw materials comprise 1275kg of phthalic anhydride, 1230kg of propylene glycol and 3kg of triphenyl phosphite of the first step material; 3650kg of maleic anhydride, 1000kg of methyl propylene glycol, 1580kg of propylene glycol, 3kg of triphenyl phosphite and 2200g of hydroquinone in the second step; 3650kg of auxiliary agent and small materials of styrene, JQ2000g, DQ800g, T504000 g, CU260g and 50kg of replenishing concentrated solution.
By adopting the technical scheme, the BMC molding resin is prepared by mixing 1275kg of phthalic anhydride, 1230kg of propylene glycol, 6kg of triphenyl phosphite, 3650kg of maleic anhydride, 1000kg of methyl propylene glycol, 1580kg of propylene glycol, 2200g of hydroquinone, 3650kg of styrene, JQ2000g, DQ800g, T504000 g, CU260g and 50kg of thickening fluid, wherein the content of each component is fixed, so that the optimal proportioning and mixing effect is achieved, and the BMC molding resin is prepared by a reaction kettle and a diluting kettle through composite stirring.
The invention also discloses a reaction kettle suitable for the BMC molding resin preparation method, and in the specific embodiment of the invention: the stirring device comprises a kettle body 1, wherein a feed inlet 2 and a discharge outlet 3 are arranged on the kettle body 1, a stirring rod 4 is arranged in the kettle body 1, a stirring motor 5 is arranged on the upper surface of the kettle body 1, the upper end of the stirring rod 4 is fixedly connected with the output end of the stirring motor 5, a first stirring component is arranged at one end, far away from the stirring motor 5, of the stirring rod 4, the first stirring component comprises a first stirring ring 6, a second stirring ring 7 and a third stirring ring 8 which are concentrically arranged and in a circular ring shape, the diameters of the first stirring ring 6, the second stirring ring 7 and the third stirring ring 8 are sequentially reduced, the upper part of the first stirring ring 6 is fixedly connected with one end, far away from the stirring motor 5, of the stirring rod 4, two first rotating connecting rods 9 are arranged on the outer ring wall of the second stirring ring 7, the two first rotating connecting rods 9 are symmetrically arranged at two sides of the outer ring wall of the second stirring rod 4 by taking the ring center of the second stirring ring 7 as, two first rotating holes 10 matched with the two first rotating connecting rods 9 are formed in the inner ring wall of the first stirring ring 6, the included angle between the connecting line between the two first rotating holes 10 and the horizontal plane is 45 degrees or 135 degrees, first bearings 11 are arranged in the first rotating holes 10, the first rotating connecting rods 9 are rotatably connected into the first rotating holes 10 through the first bearings 11, two second rotating connecting rods are arranged on the outer ring wall of the third stirring ring 8, the two second rotating connecting rods are symmetrically arranged on two sides of the outer ring wall of the third stirring rod 4 by taking the ring center of the third stirring ring 8 as a symmetry point, two second rotating holes matched with the two second rotating connecting rods are formed in the inner ring wall of the second stirring ring 7, the included angle between the connecting line between the two second rotating holes and the horizontal plane is different from the connecting line between the two first rotating holes 10 by 90 degrees, the second rotates and is provided with the second bearing in the hole, the second rotates the connecting rod and rotates in the hole through the second bearing rotation connection, the drill way department in first rotation hole 10 and second rotation hole all sets up sealing washer 12, the fixed stirring portion 13 that is provided with in one side that puddler 4 was kept away from to first agitator ring 6, the lower part of the external lateral wall of the cauldron body 1 is provided with the sampling subassembly.
By adopting the technical scheme, in the process of producing BMC (bulk molding compound) molding resin, the feed inlet 2 on the kettle body 1 is opened, the checked raw materials are sequentially put into the kettle body 1 from the feed inlet 2 of the kettle body 1, then the feed inlet 2 is closed, the stirring motor 5 on the upper surface of the kettle body 1 is started, the stirring rod 4 is driven by the stirring motor 5 to rotate, the rotating stirring rod 4 drives the first stirring component and the stirring part 13 to rotate, the first stirring ring 6 rotates coaxially with the stirring rod 4 along with the rotation of the stirring rod 4, the raw materials in the kettle body 1 are stirred by the second stirring ring 7 in the first stirring ring 6 and the stirring part 13, the first rotating connecting rod 9 on the second stirring ring 7 is mutually matched with the first bearing 11 in the first rotating hole 10, so that the second stirring ring 7 rotates along with the rotation of the first stirring ring 6 and the flowing of the raw materials by using the connecting line of the two first rotating holes 10 as a rotating shaft, the second rotating connecting rod on the third stirring ring 8 is matched with the second bearing in the second rotating hole, so that the third stirring ring 8 rotates by taking the connecting line of the two second rotating holes as a rotating shaft along with the rotation of the second stirring ring 7 and the flowing of the raw materials, the raw materials in the kettle body 1 generate different flow directions in the mixing process through the difference of the rotating directions of the first stirring ring 6, the second stirring ring 7 and the third stirring ring 8, so that the raw materials are fully mixed, sampling detection is carried out through the sampling assembly after the raw materials are fully mixed, and the discharge port 3 on the kettle body 1 is opened to discharge the raw materials after the raw materials are detected to be qualified.
In a specific embodiment of the invention: the sampling assembly comprises a discharge pipe 14 and a collecting bottle 15, the discharge pipe 14 is fixedly arranged at the lower part of the outer side wall of the kettle body 1 and is communicated with the interior of the kettle body 1, a valve 16 is arranged in the discharge pipe 14, a connecting part 17 is arranged at one end of the collecting bottle 15, a connecting pipeline is arranged in the connecting part 17 and is communicated with a bottle cavity of the collecting bottle 15, the outer diameter of the connecting part 17 is the same as the inner diameter of the pipeline of the discharge pipe 14 and is matched with the inner diameter of the pipeline, a clamping assembly is arranged on the outer side wall of the connecting part 17 and comprises a clamping block 18, a clamping block mounting cavity 19 and a plurality of springs 20, the clamping block mounting cavity 19 is arranged on the outer side wall of the connecting part 17, the vertical section of the clamping block mounting cavity 19 is in a concave shape, openings are formed in the outer side wall of the connecting part 17 at two ends of the clamping block 18, the vertical, the both ends of fixture block 18 wear out the opening at fixture block installation cavity 19 both ends respectively, the one end of spring 20 and fixture block installation cavity 19 are for the inner wall fixed connection of opening one side, and the outer wall fixed connection of opening one side is kept away from with fixture block 18 to the other end, one side that the cauldron body 1 was kept away from to discharging pipe 14 inner wall is provided with the draw-in groove 21 of mutually supporting with fixture block 18, the one end that collecting bottle 15 was kept away from to connecting portion 17 is provided with first sealing washer 22, the fixed second sealing washer 23 that mutually supports with first sealing washer 22 that is provided with on the inner wall of the pipeline of discharging pipe 14.
By adopting the technical scheme, in the process of producing BMC (bulk molding compound) molding resin, after raw materials are fully mixed, the stirring motor 5 is shut down, then one end of a fixture block on a connecting part 17 of the collecting bottle 15, which is close to the collecting bottle 15, is pressed, one end of the fixture block is pressed into a fixture block mounting cavity 19, the spring 20 is compressed, the other end of the fixture block is retracted into the fixture block mounting cavity 19, then the connecting part 17 of the collecting bottle 15 is inserted into the discharging pipe 14, after the connecting part 17 is inserted into the discharging pipe 14, the fixture block is loosened, the compressed spring 20 ejects the fixture block out of the fixture block mounting cavity 19, one end of the fixture block is positioned outside the discharging pipe 14, at the moment, one end of the fixture block, which is positioned inside the discharging pipe 14, is matched with the clamping groove 21 after being ejected by the spring 20 to fix the connecting part 17 in the discharging pipe 14, after the, then a valve 16 on a discharge pipe 14 is opened, raw materials in the kettle body 1 enter a material collecting bottle 15 through the discharge pipe 14, the valve 16 is closed after the material collecting bottle 15 is filled with the raw materials, the material collecting bottle 15 is taken down from the discharge pipe 14, the discharge pipe 14 is washed by clear water, the raw materials in the material collecting bottle 15 are poured out and detected, compared with the prior art, the sampling device is convenient to sample, the phenomenon that a large amount of air enters the kettle body 1 in the sampling process is reduced, the phenomenon that the raw materials are burnt by high temperature in the sampling process is reduced, and the sampling efficiency is improved.
In a specific embodiment of the invention: the bottleneck of the collecting bottle 15 is conical.
By adopting the technical scheme, the conical bottle mouth can reduce the raw material residue in the collecting bottle 15 when the collecting bottle 15 pours out the raw materials.
In a specific embodiment of the invention: an electric heating device 24 is fixedly arranged at the bottom of the material collecting bottle 15.
Through adopting above-mentioned technical scheme, electric heating device 24 can prevent that collection bottle 15 temperature from crossing lowly to lead to the raw materials to solidify and influence and get the material and detect, makes the raw materials keep liquid the phenomenon that the raw materials remained in having also reduced the collection bottle 15 simultaneously.
In a specific embodiment of the invention: and a pressure release valve 25 is arranged on the outer side wall of the kettle body 1.
Through adopting above-mentioned technical scheme, at the in-process of production BMC mould pressing resin, relief valve 25 on the lateral wall of the cauldron body 1 can in time open the pressure of the internal portion of the cauldron body 1 of letting out when the internal pressure of the cauldron body 1 is too big, reduces to appear because of the phenomenon that the pressure is too big leads to the cauldron body 1 to explode, has improved the security of the cauldron body 1.
The invention also discloses an operation method of the reaction kettle suitable for BMC molding resin, which comprises the following steps: the method comprises the following steps:
firstly, feeding raw materials: opening the feed inlet 2 on the kettle body 1, sequentially feeding the checked raw materials into the kettle body 1 through the feed inlet 2 of the kettle body 1, and then closing the feed inlet 2.
Secondly, stirring and mixing the raw materials: start agitator motor 5 of the 1 upper surface of the cauldron body, agitator motor 5 drives puddler 4 and rotates, and pivoted puddler 4 drives first stirring subassembly and stirring portion 13 and rotates, and first stirring subassembly rotates and stirs the raw materials in the cauldron body 1 with stirring portion 13, makes the raw materials intensive mixing.
Thirdly, sampling and detecting: after the raw materials are fully mixed, the stirring motor 5 is turned off, then the connecting part 17 of the collecting bottle 15 is inserted into the discharging pipe 14, the clamping component on the connecting part 17 is matched with the clamping groove 21 on the inner wall of the pipeline of the discharging pipe 14, the first sealing ring 22 is abutted to the second sealing ring, then the valve 16 on the discharging pipe 14 is opened, the valve 16 is closed after the collecting bottle 15 is filled with the raw materials, the collecting bottle 15 is taken down from the discharging pipe 14, the discharging pipe 14 is washed by clean water, and finally the detection is carried out in the collecting bottle 15.
Fourthly, discharging raw materials: and after the raw materials are detected to be qualified, opening a discharge port 3 on the kettle body 1 to discharge the raw materials from the kettle body 1.
Fifthly, cleaning the kettle body 1: after the raw materials are discharged, the inside of the kettle body 1 is washed by clear water and is ready for the next reaction.
By adopting the technical scheme, the mixing sufficiency of the raw materials in the reaction kettle body 1 in the stirring and mixing process is improved, so that the quality stability of the BMC (bulk molding compound) mould pressing resin is improved, and the strength and hardness of the BMC mould pressing resin are improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A preparation method of BMC molding resin is characterized in that: the method comprises the following steps:
s1: before feeding, nitrogen is introduced into the esterification reaction kettle, and the states of valves, a water outlet system and valves of a vacuum buffer tank are checked.
S2: checking the name and the quantity of the raw materials, and sequentially feeding the raw materials according to a feeding sequence after the raw materials are accurately confirmed; firstly, liquid alcohol is added, after the alcohol is added, the mixture is preheated to 80-90 ℃, and then solid materials (neopentyl glycol, phthalic anhydride and triphenyl ester are added in sequence) are added.
S3: after the feeding is finished, adding corresponding auxiliary agents and small materials, slowly opening a heating (large and small) oil valve to start heating, observing the reaction condition of the materials in the reaction kettle, taking emergency measures in time when an abnormal condition is found, and reporting to a production department.
S4: the first step is that the material is heated to water, and then the temperature of the water is slowly heated to 195 +/-1 ℃, the process needs about 5 hours, the temperature of the top of the tower is controlled not to exceed 103 ℃ in the heating process, nitrogen (3-5 m3/h) is introduced in the heating process to reach the required temperature (195 ℃), and then the sampling acid value is measured to be 30-40 mgKOH/g, so that the material can be cooled.
S5: cooling the material to below 150 deg.C to prepare the second step material and adjuvant (the feeding sequence is propylene glycol, liquid anhydride, triphenyl ester and hydroquinone).
S6: and (2) after the materials are fed, heating to 162 +/-2 ℃ to discharge water, carrying out heat preservation reaction for 0.5 hour after water discharge, heating to 208 +/-1 ℃ to preserve heat, carrying out heat preservation at a constant speed for about 6 hours after water discharge, introducing nitrogen gas for 3-5 m3/h in the heating process, controlling the temperature at the top of the tower to be not more than 103 ℃, preserving heat for about 3 hours, and measuring the acid value.
S7: when the acid value is 62-68 mgKOH/g, the viscosity of the polyester vertebral plate at 150 ℃ is as follows: 1.0-1.4P, starting vacuum, wherein the vacuum time is about 4-4.5 hours (the vacuum degree is more than-0.092 Mpa), the acid value after vacuum is 26-28 mgKOH/g, and the viscosity of a polyester vertebral plate at 150 ℃ is as follows: 10.5 to 11P, cooling to 180 +/-1 ℃ after the product is qualified, adding JQ and PQ hydroquinone, and continuously cooling the material to 158 +/-2 ℃ until the material temperature is reached, so that dilution can be carried out. (the time from the addition of JQ to the start of thinning is not less than 40 minutes)
S8: and before diluting, ensuring that the styrene is injected into the diluting kettle, starting stirring the diluting kettle, adding DQ and T50 small materials in advance, then starting diluting, controlling the diluting flow and the diluting kettle material temperature in the diluting process, controlling the highest material temperature of the diluting kettle at 80-83 ℃ after diluting is finished, and optimally controlling the diluting time at 40-60 minutes.
S9: cooling to about 70 ℃ after the dilution is finished, adding copper naphthenate, dehydrating for 40 minutes in vacuum, continuously cooling to about 65 ℃, sampling, detecting, filtering and packaging after the product is qualified.
2. The method of claim 1, wherein the BMC molding resin comprises: the raw materials comprise 1275kg of phthalic anhydride, 1230kg of propylene glycol and 3kg of triphenyl phosphite of the first step material; 3650kg of maleic anhydride, 1000kg of methyl propylene glycol, 1580kg of propylene glycol, 3kg of triphenyl phosphite and 2200g of hydroquinone in the second step; 3650kg of auxiliary agent and small materials of styrene, JQ2000g, DQ800g, T504000 g, CU260g and 50kg of replenishing concentrated solution.
3. A reaction vessel suitable for the BMC molding resin preparation method of claim 1, characterized in that: the stirring device comprises a kettle body, wherein a feed inlet and a discharge outlet are arranged on the kettle body, a stirring rod is arranged in the kettle body, a stirring motor is arranged on the upper surface of the kettle body, the upper end of the stirring rod is fixedly connected with the output end of the stirring motor, a first stirring assembly is arranged at one end, far away from the stirring motor, of the stirring rod, the first stirring assembly comprises a first stirring ring, a second stirring ring and a third stirring ring which are concentrically arranged and in a circular ring shape, the diameters of the first stirring ring, the second stirring ring and the third stirring ring are sequentially reduced, the upper portion of the first stirring ring is fixedly connected with one end, far away from the stirring motor, of the stirring rod, the outer ring wall of the second stirring ring is provided with two first rotating connecting rods, the two first rotating connecting rods are symmetrically arranged on two sides of the outer ring wall of the second stirring rod by taking the center of the second stirring ring as a symmetry point, two first rotating holes matched with the two first rotating connecting rods are arranged on the inner ring wall of the first stirring, an included angle between a connecting line between the two first rotating holes and a horizontal plane is 45 degrees or 135 degrees, a first bearing is arranged in each first rotating hole, the first rotating connecting rods are rotatably connected in the first rotating holes through the first bearings, two second rotating connecting rods are arranged on the outer ring wall of the third stirring ring, the two second rotating connecting rods are symmetrically arranged on two sides of the outer ring wall of the third stirring rod by taking the ring center of the third stirring ring as a symmetrical point, two second rotating holes matched with the two second rotating connecting rods are arranged on the inner ring wall of the second stirring ring, the included angle between the connecting line between the two second rotating holes and the horizontal plane is 90 degrees different from the connecting line between the two first rotating holes, a second bearing is arranged in each second rotating hole, the second rotating connecting rods are rotatably connected in the second rotating holes through the second bearings, and sealing rings are arranged at the orifices of the first rotating holes and the second rotating holes, one side of the first stirring ring, which is far away from the stirring rod, is fixedly provided with a stirring part, and the lower part of the outer side wall of the kettle body is provided with a sampling assembly.
4. The kettle of claim 3, wherein the kettle comprises: the sampling assembly comprises a discharging pipe and a collecting bottle, the discharging pipe is fixedly arranged at the lower part of the outer side wall of the kettle body and is communicated with the interior of the kettle body, a valve is arranged in the discharging pipe, a connecting part is arranged at one end of the collecting bottle, a connecting pipeline is arranged in the connecting part and is communicated with the bottle cavity of the collecting bottle, the outer diameter of the connecting part is the same as the inner diameter of the pipeline of the discharging pipe and is matched with the inner diameter of the pipeline of the discharging pipe, a clamping assembly is arranged on the outer side wall of the connecting part and comprises a clamping block, a clamping block mounting cavity and a plurality of springs, the clamping block mounting cavity is arranged on the outer side wall of the connecting part, the vertical cross section of the clamping block mounting cavity is in a concave shape, openings are formed in the outer side wall of the connecting part at two ends of the clamping block, the vertical cross section of the clamping block is in, one end of the spring is fixedly connected with the inner wall of the clamping block mounting cavity on one side of the opening, the other end of the spring is fixedly connected with the outer wall of the clamping block on one side of the opening, the clamping groove matched with the clamping block is formed in one side, away from the kettle body, of the inner wall of the discharge pipe, one end, away from the material collecting bottle, of the connecting portion is provided with a first sealing ring, and a second sealing ring matched with the first sealing ring is fixedly arranged on the inner wall of the pipeline of the discharge pipe.
5. The kettle of claim 4, wherein the kettle comprises: the bottleneck of the collecting bottle is conical.
6. The kettle of claim 5, wherein the kettle comprises: and an electric heating device is fixedly arranged at the bottom of the material collecting bottle.
7. The kettle of claim 3, wherein the kettle comprises: and a pressure release valve is arranged on the outer side wall of the kettle body.
8. A method of operating a BMC molding resin reaction vessel adapted for use with any of claims 3-7, comprising: the method comprises the following steps:
firstly, feeding raw materials: and opening a feed inlet on the kettle body, sequentially putting all the checked raw materials into the kettle body from the feed inlet of the kettle body, and then closing the feed inlet.
Secondly, stirring and mixing the raw materials: the agitator motor of start-up cauldron body upper surface, agitator motor drive the puddler and rotate, and the pivoted puddler drives first stirring subassembly and stirring portion and rotates, and first stirring subassembly rotates and stirs the raw materials in the cauldron body with stirring portion, makes the raw materials intensive mixing.
Thirdly, sampling and detecting: after the raw materials intensive mixing, turn off agitator motor, then insert the connecting portion of collecting bottle discharging pipe, make joint subassembly on the connecting portion mutually support with draw-in groove on the discharging pipe pipeline inner wall, and make first sealing washer and second sealing washer butt, then open the valve on the discharging pipe, close the valve after filling with the raw materials in waiting the collecting bottle, take down the collecting bottle on by the discharging pipe, and wash the discharging pipe with the clear water, detect in the collecting bottle at last.
Fourthly, discharging raw materials: and after the raw materials are detected to be qualified, opening a discharge hole on the kettle body to discharge the raw materials from the kettle body.
Fifthly, cleaning the kettle body: after the raw materials are discharged, the interior of the kettle body is washed by clear water and is ready for the next reaction.
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Application publication date: 20200609 |