WO2007020940A1

WO2007020940A1 - Multistage gear processing equipment

Info

Publication number: WO2007020940A1
Application number: PCT/JP2006/316099
Authority: WO
Inventors: Kosuke Uchiyama
Original assignee: Kosuke Uchiyama
Priority date: 2005-08-17
Filing date: 2006-08-16
Publication date: 2007-02-22
Also published as: JP5563736B2; KR20080039955A; JPWO2007020940A1; KR101352346B1

Abstract

Equipment for processing a substance mixed with gas as fluid under critical state by kneading/compressing it continuously. Two stages or more of gear transporting sections having different gear dimensions or different capacities are provided, pressure difference of gas compression is controlled by the difference in fluid transportation capacity between two continuous stages of gear transporting section, or a part of transportation fluid is fed reversely thus keeping the substantial transportation capacity at a constant level. A plurality of paired gears are preferably provided between the two continuous stages of gear transporting section.

Description

Specification

Multi-stage gear type processing machine

Technical field

[0001] The present invention relates to an apparatus for compressing a substance together with, for example, carbon dioxide gas as a fluid in a critical state, that is, processing such as kneading, decomposition, extraction or chemical synthesis under supercritical or subcritical carbon dioxide gas About.

Background art

Numerous substance mixing, substance extraction, substance decomposition, and chemical synthesis using supercritical carbon dioxide have already been proposed, and in particular in the field of extraction.

[0003] For example, Patent Document 1 discloses carbon dioxide gas in a continuous processing method in which liquid food or liquid chemical is subjected to enzyme deactivation, sterilization, deodorization, extraction processing, etc. using a supercritical fluid or subcritical fluid. A compression process in which a liquid raw material is injected into a suction process or a compression process of a compressor serving as a working medium and compressed together with carbon dioxide, and carbon dioxide and the liquid raw material are brought into direct contact to form a high-pressure gas-liquid mixed fluid in a critical state; Liquid gas separation process that separates high pressure carbon dioxide gas and liquid substance from high pressure gas-liquid mixed fluid in a critical state into high pressure carbon dioxide gas, and high pressure that melts the separated liquid substance It has been proposed to use a decompression process in which the carbon dioxide gas is rapidly decompressed to discharge the low-temperature carbon dioxide gas by releasing the criticality and perform enzyme deactivation treatment, pasteurization treatment, and flavor extraction treatment.

[0004] In this proposal, in order to supply the raw material liquid to the compressor by a pump and to achieve the supercritical condition with the separator, a large number of devices are required, and the capital investment is excessive, which is economically favorable. Absent. In addition, the operating conditions are limited to low temperatures, and there is a drawback that the application range is narrowed.

[0005] In Patent Document 2, the recovered polyester product is broken into flakes, washed, and devolatilized and dried with water in a pre-process screw kneading extruder, and added with a modifier and a catalyst. There has been proposed a method and an apparatus for recycling recovered polyester products that are subjected to a quality reaction and further subjected to foam extrusion while adding a supercritical fluid with a post-process screw extruder.

[0006] In this proposal, a screw extruder is used. It is assumed that foamed products are produced by injecting supercritical carbon dioxide in the process, and there is no reaction in supercritical carbon dioxide. In addition, because of the screw type, gas leakage occurs, and it is not possible to process the gas in a low-viscosity material.

[0007] Patent Document 3 proposes an extruder in which at least two gear pumps are connected and unmelted vinyl chloride powder is melted and mixed in the gear pump.

[0008] In this proposal, it is preferable to connect two or more gear pumps in view of the kneading effect, and there is no description of a control method in the case where the number of rotations between the force gear pumps is different. When gear pumps of the same capacity are connected at the same speed, it is possible to operate without causing abnormal pressure between the connected gear pumps. However, when gear pumps with different capacities are connected, for example, when a small capacity gear pump is connected next to a large capacity gear pump, an abnormally high pressure is generated between the gear pumps, and the large capacity gear pump is excessive. The road is loaded, the shear pin flies, and you cannot actually drive.

Patent Document 1: Japanese Patent Application Laid-Open No. 2002-204942

Patent Document 2: Japanese Patent Laid-Open No. 2000-264998

Patent Document 3: Japanese Patent Laid-Open No. 11-34045

Disclosure of the invention

Problems to be solved by the invention

[0009] An object of the present invention is to provide an apparatus capable of performing processing such as decomposition, mixing, or extraction of a substance with good operability using supercritical or subcritical gas.

[0010] In the present invention, the above-mentioned problem has been solved by installing a multi-stage gear unit equipped with a method for controlling the pressure of gas compression of a substance in which gas is mixed, or controlling the backflow of a part of the transferred substance. .

[0011] That is, the apparatus of the present invention is a processing apparatus for continuously kneading a substance in which gas is mixed, and includes gear-type transfer units having different gear dimensions (that is, different transfer unit capacities).

Two or more stages are provided, and the pressure difference in gas compression is controlled by the difference in transfer capacity between two successive gear-type transfer parts, or a part of the transferred substance is made to flow backward to make the actual transfer capacity constant. To do.

[0012] Hereinafter, the temperature and temperature at which a gas-containing substance passes through the gear-type transfer unit within a certain time will be described. The sum of the volume of the substance and gas at the pressure and pressure is referred to as “transfer capacity”, and the transfer capacity capacity of the gear-type transfer part is referred to as “transfer part capacity”. The sum of the volume of substances and gases at the same temperature and the equivalent pressure of 1 atm is referred to as “substantial transfer capacity”.

[0013] It should be noted that the continuous two-stage gear-type transfer unit is provided with a plurality of, preferably 2 to 4, gears paired between them, and is transferred by each gear-type transfer unit. The transfer capacity varies depending on the rotation speed and dimensions (module, pitch circle diameter, gear thickness, etc.) of the gear type transfer section. The capacity of the transfer section is approximately proportional to the product of the number of rotations of the gear, the module, the pitch circle diameter, and the gear thickness. In practice, however, the gas is compressed and adjusted so that the actual transfer capacity is constant. It is better to apply a method of adjusting the force by the back flow from the outlet side to the inlet side. The powerful gear-type transfer unit is, for example, preferably provided following the extrusion screw, because the first gear transfer unit capacity of the gear transfer unit preferably smaller than the second gear transfer unit capacity is The pressure during that time can be made negative. By providing a gear having a smaller transfer section capacity than the second gear behind the second gear, it is possible to increase the pressure or to obtain a desired effect.

[0014] In the apparatus of the present invention, a low-viscosity raw material can be continuously processed, and a high-pressure condition of supercritical or subcritical gas can be generated by the gear-type transfer unit.

[0015] The apparatus of the present invention is an extruder or an injection molding machine, and at the same time, continuously decomposes, mixes or extracts a substance in a supercritical or subcritical carbon dioxide gas and performs a wide range of operating conditions. This is a general-purpose chemical equipment that can be used and has many inexpensive processes, making it inexpensive and economical. In addition, gear-type transfer units can be stacked vertically, and the installation area can be reduced with a compact device.

Brief Description of Drawings

FIG. 1 is an explanatory diagram of a gear pump structure of a step-down unit.

FIG. 2 is an explanatory diagram of a gear pump structure of a boosting unit.

FIG. 3 is an explanatory diagram of a gear pump structure of a kneading part.

FIG. 4 is an explanatory view showing the structure of an orifice part.

FIG. 5 is an explanatory diagram showing a structure of a pressure control unit. [6] The structure of the multi-stage gear extruder is shown. (I) shows the front part and (II) shows the rear part.

[Fig. 7] Shows the structure of a multi-stage gear type foam injection molding extruder.

FIG. 8 shows a structure in which multi-stage gear extruders are arranged horizontally, (1) is a plan sectional view, and (2) is a longitudinal sectional view.

[9] This is a plan sectional view of a structure in which multi-stage gear extruders are arranged in an arc. Explanation of symbols

1 cylinder

2 shaft

3 shaft

4 shaft

5 screw

6 Difficult

7 Conduction relay gear

8 Honoichi

9 Orifice

10 Vent hole

11 Dice

12 nozzles

13 Flow passage

14 Return passage

15 arrows

16 Servo 'motor

17 Servo 'Amplifier

18 sword electrical signal

19 Oil pressure gauge

20 Pressure gauge

21 Pressure reducing valve 22 Check valve

23 Melting section

24 Pressurization section

25 Supercritical section

26 Orifice section

27 No-flight section

28 Pressure adjustment section

29 Gas injection section

30 Boosting interval

31 Supercritical section

32 Buck section

BEST MODE FOR CARRYING OUT THE INVENTION

[0018] The present invention will be described according to an example shown in the drawings.

The apparatus of the present invention uses a multi-stage gear-type transfer unit that combines gears as shown in FIGS. 1, 2, and 3, and processes a substance mixed with gas transferred between them as a fluid in a critical state. Is. For example, the twin-shaft horizontal gear extruder in Fig. 6 is equipped with a multi-stage gear-type transfer section following the twin-screw extrusion screw of the raw material supply section, and inside the cylinder 1 heated by an electric heater, An A-axis screw and a B-axis screw are provided, and the resin raw material supplied from the hopper 8 is melted while being transferred, and the molten resin in the melt zone 23 is converted into the next gear as shown in FIG. Flow into. The gear T1 and the subsequent gear T2 have a relationship of T1 <T2, and the gear shown in Fig. 1 has a pressure-lowering section X, and the gas is compressed by the supply pressure set by the pressure-reducing valve 21 and the gear thickness is reduced. A certain amount of volume transfer gas corresponding to the dimensional difference (Τ2-T1) is injected. The fluid after gear Τ2 is a mixture of gas and grease. Therefore, the gas injection amount is larger as the supply pressure set by the pressure reducing valve 21 is higher. This gas is degassed through a vent hole 10 sucked by a vacuum pump. In this example, the screw may be a single axis with two axes.

FIG. 1 shows a gear pump structure of the step-down portion X, and FIG. 1 (1) shows a plan view. (1) in Fig. 1 is a cross-sectional view of the axial force on the Out side, and (3) and (4) in Fig. 1 are side views. The As shown in the drawing, the A-axis shaft 2 and the B-axis shaft 3 pass through the inside of the cylinder 1, and the gears T1 and T2 having different thicknesses are fixed to the respective shafts so as to be fixed to each other. It constitutes a set of gear pumps. The A-axis and B-axis shafts 2 and 3 are driven in the direction of rotation as indicated by the arrow 15, and the grease filled in the flow passage 13 is conveyed to the Out side from the In side cover illustrated by the gears. . Under the condition that the thickness of the gears T1 and T2 is TKT2, it acts on the tendency to increase the transfer capacity of the gear T2 over the transfer capacity of the gear T1.

[0020] Next, an example in which the substance is a melt of thermoplastic resin and the gas is carbon dioxide will be described as an example. In FIG. 1, when a fluid containing a mixture of resin and gas flows from In, the transfer capacity of the gear T1 corresponds to the sum of the volume of the resin and the volume of gas compressed by pressure P1. The transfer capacity of the gear T2 is equivalent to the sum of the volume of the resin that has passed through the gear T1 and the volume of the gas compressed by the pressure P2. Under the condition that the gear thickness is TKT2, the transfer capacity is greater with the gear T2 than the gear T1, and the pressure P1> P2. The structure of (3) in Fig. 1 is used in the first stage of the multi-stage gear group mainly for the purpose of gas injection. In the case where a fluid containing only a resin containing no gas flows into the In force, the gas volume compressed to the carbon dioxide pressure P2 supplied to the Gas injection locus regardless of the PI is equivalent to the difference in gear thickness dimension (T2-T1). Become volume. In this case, it is not necessary for the fluid flowing from In to be only grease, and even if it is a mixture of grease and gas, carbon dioxide is injected under the balanced conditions of gear Tl, gears T2, PI and Ρ2. Things come out. The structure of (4) in Fig. 1 is used at the end of the multi-stage gear group mainly for the purpose of reducing the pressure of the fluid mixed with gas to the supercritical region force and subcritical region.

[0021] Fig. 2 shows the gear pump structure of the boosting unit Y. Fig. 2 (1) is a plan view, Fig. 2 (2) is a cross-sectional view seen from the axial direction of Fig. 2 (3 ) Shows a side view. The fluid flowing from In is, for example, a sufficiently compressible fluid in which coagulate and gas are mixed. Even if the gear thicknesses are Tl>T2> T3, the actual transfer capacity is the same for each gear, so the internal pressure in the flow passage 13 is increased to <1 <Ρ2, and the pressures of Pl and それぞれ 2 respectively. As a result, the fluid is compressed and the transfer capacity is balanced. Assuming that the actual transfer capacity is unknown and the pressure of fluid flowing from In is very high, it is not always PC P1 under the condition of T1> T2, and W cannot be defined as a booster. Usually, at the design stage, the actual transfer capacity and Ρ0 are known as design values. The booster can also be configured by a combination of stepped gears. For the reasons described above, Fig. 2 consists of a combination of three gears. The structure in Figure 2 is mainly used for the following two applications:

[0022] Application of the structure of Fig. 2 As an example, the structure of Fig. 1 (3) is installed for the purpose of raising the pressure to the supercritical region in the next stage where carbon dioxide gas is injected. In this case, the first stage of the booster can be considered as gear T2 in FIG.

[0023] As an example of the use of the structure of FIG. 2, there is a blending example (for example, a mixture of 58% starch and 42% water by weight) to sufficiently pregelatinize starch. When the water is carbonated water in which carbon dioxide gas is previously dissolved in water, for example, in the apparatus shown in FIG. 6, when this mixture is supplied from the hopper 8, the screw 5 under the hopper is sufficiently eaten by the starch in the dilatant flow. Using a 2-shaft paddle screw, the water turns into steam during overheating transport to the first stage of the multi-stage gear. Since carbon dioxide is already contained in carbonated water, gas injection is unnecessary, and the structure shown in Fig. 2 is used to boost the pressure from the first stage of the multi-stage gear to the supercritical region.

FIG. 3 shows a gear pump structure of the kneading part Z, and FIG. 3 (1) shows a plan view. Figure 3

(2) is a cross-sectional view seen from the Out side axial direction, and (3) in FIG. 3 is a side view. (4) in Fig. 3 shows the movement relationship between the gears attached to the shafts 2, 3, and 4 of the A, B, and C axes and the fluid. As shown in Fig. 3 (2), the flow path on the outer periphery of the A-axis gear, a part of the fluid passes through the outer periphery of the A-axis gear from the Out side and is supplied to the inlet of the C-axis gear. From the exit of the gear, return to the In side through the return path 14 around the outer periphery of the A-axis gear. This amount of backflow is shown as (4) Koko FB in Fig. 3. It is characterized by an excellent kneading effect depending on the amount of FB, and also by stabilizing the pressure on the In side and Out side. In addition, as shown in (5) of Fig. 3, it is possible to use four gears by providing a gear on the D-axis that works in the same way as a C-axis gear. The amount of reverse flow with the C-axis gear is indicated as FBC, and the amount of reverse flow with the D-axis gear is indicated as FBD. This pair of gears can be used for both the pressure raising part, the pressure reducing part and the part where the pressure is balanced. The kneading and dispersing effect is extremely excellent.

[0025] Fig. 4 shows the structure of the orifice part. Installed mainly in the supercritical section, the fluid flows from In and passes through the narrow groove of the orifice 9 to the flow path force Out. The fluidity of the fluid in the section where the gas is in the supercritical state is high. And the dispersion effect becomes even higher.

FIG. 5 shows the structure of the pressure control unit. Mainly the pressure control unit is convenient for multi-stage gear type machining equipment for research and development use In the production machine, the step-down unit X with the gear fixed to the A-axis and B-axis shown in Fig. 1 is simple, and the pressure control unit Do not need. The purpose of providing a pressure control unit is mainly to investigate the relationship between the amount of carbon dioxide added and the pressure, etc., on the degree of chemical reaction, the degree of kneading and dispersion, or to determine the specifications of the production machine. It becomes. The fluid passage is blocked at the non-flight section 27 without a screw groove in the rear stage of the orifice in the supercritical section of the screw, the bypass passage of the flow passage 13 is provided, and the gear 6 driven separately from the screw 5 by the servo 'motor 16 To the latter part of the no-flight section 27. Normally, the gear 6 comprises the step-down part X with two stages of gears. If the rotation speed of the servo motor is lowered, the pressure at the mounting portion of the grease pressure gauge 19 will increase, and if the rotation speed of the servo motor is increased, the pressure at the mounting portion of the grease pressure gauge 19 will decrease. The servo motor 16 is driven by the servo amplifier 17, and the electrical pressure signal 18 is fed back from the grease pressure gauge 19 in response to the pressure command commanded to the servo amplifier so that the servo motor 16 approaches the pressure set value. · The motor rotation speed is controlled to configure automatic pressure control.

FIG. 6 shows an example of a multi-stage gear extruder. Resin is supplied from the hopper 8 and heated by the heater, and the resin is heated and melted by the A-axis and B-axis twin-screws 5 installed in the cylinder 1 as shown in Fig. 1. The first stage of a multi-stage gear. Although this example consists of two axes, the objective can be achieved with one axis. At the rear of the first stage of the multi-stage gear, the carbon dioxide gas cylinder pressure is also reduced by the carbon dioxide gas pressure reducing valve 21 and supplied through the check valve 22. The pressure of the supplied carbon dioxide gas is confirmed with a pressure gauge 20. The carbon dioxide gas is compressed and kneaded by the screw installed in the supercritical section 25 through the pressurizing section 24 together with the fat carried by the screw 5, and the carbon dioxide gas becomes supercritical. The next orifice section 26 is reached. The mixture of gas and gas that has passed through the orifice section 26 is blocked in the non-flight section 27 in the next stage, and flows into the pressure adjustment section 28 by the servo motor. The fluid that has passed through the pressure adjustment section flows into the screw section where the vent hole 10 is installed. At this time, the carbon dioxide gas is reduced in pressure from the supercritical state to the subcritical state. The mixed fluid of oil and gas is sucked through the vent hole connected to the vacuum pump and degassed. To do. Vent hole force The latter stage reaches the die 11 with the same structure as a general extruder, and the fluid (resin) is cooled in a strand water tank and cut with a strand cutter. Cut with a hot cutter or submerged cutter, etc. I will be deceived. In some cases, it can be taken out in liquid form. Although the first to third gears are illustrated in the pressurizing section 24, the first and second gears are the step-down portion X described in FIG. 1, and the second and third gears are illustrated. The gear is different in figure from the booster Y described in Fig. 2, but the transfer unit capacity of three gears (explained with the kneading unit Z in Fig. 3) forming the third pair and forming the backflow unit. Is smaller than the capacity of the second transfer section, and the gas is further compressed to form the pressurizing section Y.

FIG. 7 shows an example of a multi-stage gear type foam injection molding machine / extruder. The rosin raw material is supplied from the hopper 8 and melted while passing through the screw 5 installed in the cylinder 1 heated by the heater. The purpose of the screw is to melt either uniaxial or biaxial, and either may be used. The melted resin reaches the gas injection section 29 (step-down section X as shown in FIG. 1) arranged at the first stage of the multi-stage gear section. In this section, gas is mixed into the resin and transferred to the pressurizing section 30 arranged in the next stage. In this example, a method of combining three gears as shown in (1) of FIG. 3 is employed so that pressurization and kneading are simultaneously performed. The fluid is then transferred to the supercritical section 31, and the gas mixture enters the details of the grease. It is convenient to monitor the supercritical pressure by attaching a grease pressure gauge 19 to this part. Next, the grease mixed with the gas passes through the pressure-lowering section 32 and is injected into the mold of the injection molding machine through the nozzle 12 at the tip. The nozzle has a well-known mechanical nozzle structure that can be discharged from the nozzle when pressed against the mold.

It is also possible to attach a round die or a T die instead of the nozzle and continuously foam. The illustration is an example of the apparatus of the present invention, and the number of gear stages is not necessarily limited to the illustrated number of stages.

FIG. 8 shows an example of a multi-stage gear extruder in which multi-stage gears are arranged horizontally. In FIG. 8, (1) is a plan view and (2) is a side view. The gear thickness is T1 <T2>T3> T4 The gear thickness can be selected and arranged as appropriate according to the purpose of use. Similarly, Fig. 9 shows an example of a multi-stage gear extruder with multi-stage gears arranged in an arc. The difficulty in arranging multi-stage gears in a horizontal arrangement or arc arrangement is the seal of the gear shaft, and the higher the pressure side, the more likely the seal will be broken. . In the present invention, this problem is solved by providing the conductive relay gear 7. By installing conductive relay gears in a horizontal array or circular arc arrangement, the complexity of the seal is eliminated, making it compact and ideal for various supercritical compounds for laboratory use, supercritical extraction and supercritical reaction testing machines. Became.

[0030] In order to obtain a gas-mixed substance, for example, in the apparatus of FIG. 6, the gas is supplied through the check valve 21 through the check valve, but the gas mixed in the resin is injected. Sometimes it is not necessarily a gas. It may be liquid when injecting. For example, even if water is added to rosin or starch from the hopper 8 and water vapor is generated in the middle of the transfer by the screw to form a fluid in which gas is mixed, a liquid such as gas-injected rocker is also added, It may be a fluid mixed with gas by vaporizing with the internal heat of the multi-stage gear group. That is, in the present invention, a state where a gas component is mixed in a fluid passing through the multi-stage gear group is treated as a substance containing gas or a gas-containing substance.

[0031] A die is generally used for the outlet of the apparatus of the present invention. The die hole and the shape of the die are appropriately selected according to the following steps. For example, if the next process is film or sheet production, the shape of the die hole can be made into a slit shape, and the film can be continuously produced. Also, if the next step is discontinuous, the processed material is taken out in the shape of a rope and cut with a cutter to produce pellets, extruded into a sheet to produce square pellets, or round pellets with a hot cutter or underwater cutter. Can also be manufactured. In some cases, it can be taken out in liquid form.

[0032] In some cases, the gear type machining apparatus of the present invention may be incorporated into an extrusion screw as a part of a kneading part such as an injection molding machine, an injection blow molding machine, an inflation apparatus, or a T die. Further, the gear type carriage device of the present invention can be connected in a vertically stacked manner by combination with a mandrel. By stacking vertically, the installation area of the entire processing device can be made smaller than that of a general screw extrusion kneader.

[0033] Unlike the gear-type metering pump that is generally used, the gear-type transfer unit used in the present invention focuses on the mixing effect rather than the metering. The gear shape of the gear-type transfer unit changes the center elasticity depending on the size of the leading end R of the gear. The difference in the angle between the tangent line and the center line of the gear groove changes the flow velocity of the material in the gear. The material in the gear groove by rotating the gear Will be mixed and mixed. By roughening the gear and housing surface shape, the measuring ability is reduced, but this elastic force can be increased. It is the same as a general gear pump that the metric changes depending on the volume of the gear groove and the gear speed.

[0034] It is also possible to install the gear-type transfer unit and the screw unit separately. In this case, the groove of the gear-type transfer unit gear can be installed vertically so as to be orthogonal to the screw shaft. Further, it is preferable that the gear-type transfer unit is incorporated as a module to facilitate compatibility. This is the same as the case of the horizontal type, and the same module replacement method as that used in a general twin-screw extruder. This is because the viscosity varies depending on the material used, so even with the same gear 'clearance, the reverse flow resistance varies depending on the viscosity, making it easier to select the desired pressure and the required shear strength. . Module 'systems are also advantageous for equipment cleaning.

[0035] Supercritical or subcritical gas chemistry includes chemical decomposition such as hydrolysis, alcoholysis, enzymatic decomposition, mixing of fine particles without surface treatment, mixing of liquid and polymer, insoluble polymer without using compatibilizer Examples include chemicals such as mixing, solvent extraction, and steam extraction. Catalysts, auxiliary materials, and the like may be quantitatively supplied by a plunger pump, a gear pump, or the like by a low pressure gas supply unit that may be supplied quantitatively as appropriate, or by liquid injection. Supercritical or subcritical gas may use low molecular weight compounds such as carbon dioxide, methanol, acetone, nitrogen gas, and water. Among them, carbon dioxide is often used because the critical conditions are mild and explosive. It is done.

[0036] Examples of hydrolysis include, for example, starch, kenaf, nocose, cellulose, protein, fat and the like, which are decomposed into polysaccharides, oligosaccharides, monosaccharides, amino acids, alcohols and the like. As catalysts, acids are used for sugars, and alkalis or enzymes such as amylase, peptidase, and lipase are used for proteins. The supercritical conditions of carbon dioxide gas are 31 ° C and 7 MPa, but when using an enzyme as a catalyst, it is preferable to operate in a temperature range where the enzyme is not deactivated, for example, 35 to 40 ° C and 7 MPa or more. When an acid or alkali is used as a catalyst, it is preferable to increase the temperature because reaction efficiency can be improved and productivity can be improved.

[0037] As an example of alcoholysis, for example, a so-called PET bottle is collected, and the pulverized flakes are supplied to the chemical action device of the present invention with flakes and methanol, and polyethylene terephthalate is metabolized. It can be alcoholicized with anol and recovered as terephthalic acid methyl ester. After rectification and removal of impurities, polyethylene terephthalate can be produced by polymerizing methyl terephthalate again. Also, ethylene diol can be used in place of methanol and recovered as bishydroxyethylene terephthalate, and polyethylene terephthalate can be produced in the same manner. Increasing the temperature of alcoholysis is preferable because it increases reaction efficiency and improves productivity.

[0038] As an extraction example, for example, orange peel is directly supplied to the processing apparatus of the present invention, and limonene can also be extracted from the orange peel. Increasing the extraction temperature to near the boiling point of limonene is preferable because it increases the extraction efficiency and improves the productivity. The extracted crude limonene is rectified to improve purity and used.

[0039] As an example of mixing, for example, in order to improve the heat resistance of biodegradable polylactic acid, inorganic fine particles can be supplied to the processing apparatus of the present invention as a crystallization nucleating agent to produce pellets. By using the processing apparatus of the present invention, the inorganic fine particle crystallization nucleating agent is supplied in an aqueous dispersion, mixed in a state in which polylactic acid is hydrolyzed to a low molecular weight under a carbon dioxide subcritical condition, and then dehydrated and condensed. In addition, since the dispersion is good, transparent polylactic acid pellets can be produced.

[0040] Examples of foaming include, for example, gas such as carbon dioxide and nitrogen gas, volatile substances such as butane and pentane, injection of reduced pressure, and thermochemical foaming agent such as diazo compound mixed and injected with hopper force. By such means, it can be incorporated into devices such as extrusion foaming and injection foaming. As an example, Fig. 7 shows an example of a multi-stage gear type foam injection molding machine / extruder. In this case, it can be incorporated into a general plunger type injection molding machine.

Example 1

[0041] In this example, the multistage gear extruder of the present invention shown in Fig. 6 was used. In order to handle raw materials with high water content, a single screw with a length of 50 mm, a length of 350 mm and a biaxial paddle screw at the bottom of the feed hopper was used, followed by a 400 mm long single screw. The multi-stage gear used all three stages, and the multi-stage gear driven by the servo 'motor used all two stages. The dimensions of the main part of the gear are described below. Only the dimension of the gear thickness of the A-axis and B-axis (hereinafter referred to as “tooth thickness”) is described, the tooth thickness of the C-axis is described, and the stage is described as the step-down unit X or the step-up unit Y The stage with the tooth thickness on the C-axis is the structure shown as the kneading part Z. The The pressure described next corresponds to the inlet side pressure described in the next stage as the outlet side pressure in the indicated stage, and the unit is (MPa).

The pitch circle diameter of all gears is 46mm and module 2 is adopted.

1st stage A-axis, B-axis tooth thickness 87mm 0.88 (measured value)

Second stage A-axis and B-axis tooth thickness 92mm 5. 29 (design value)

3rd stage A-axis, B-axis tooth thickness 48mm ZC-axis gear 20mm 8. 82 (design value)

Servo 'motor drive' pressure controller

1st stage A-axis and B-axis tooth thickness 20mm 8.8 (measured value)

Second stage A-axis and B-axis tooth thickness 28mm 4. 41 (design value)

Using a device consisting of a die with a round hole nozzle, underwater cutter and dryer

[0042] The following operating conditions were balanced at an extruder shaft speed of 80 rpm and a servo motor speed of 120 rpm. The temperature set by the heater is set to 160 ° C only under the inlet hopper, the set temperature of each part is set to 230 ° C, and the raw polylactic acid and 5% by weight mica water dispersion raw material ratio are blended. Supplied with. The gas injection loca was also injected with carbon dioxide reduced to 0.88 MPa with a pressure reducing valve. The indication pressure of the oil pressure gauge in the pressure adjustment part by the servo 'motor is 8.8 MPa of carbon dioxide gas supercritical, and the residence time to reach the pressure adjustment part gear is about 20 seconds (calculated value). The molecular weight of polylactic acid was recovered by reducing the pressure of the water pump at the flat screw vacuum vent. It is clear that the resulting pellets are transparent and dispersible at the nano level despite containing inorganic fine particles.

Example 2

[0043] In this example, the same multistage gear extruder as shown in Fig. 6 was used.

[0044] The following operating conditions were balanced at an extruder shaft speed of 80 rpm and a servo motor speed of 120 rpm. The temperature set by the heater is set to 160 ° C only under the inlet hopper, the temperature set for each part is set to 190 ° C, the raw material polylactic acid is 89.3% by weight, and the starch aqueous dispersion (solid content is 50% by weight). Were fed and fed at 30 kgZ hours. Carbon dioxide gas was decompressed to 0.88 MPa from the gas inlet and injected. Servo 'Motor pressure adjustment The indicated pressure of the oil pressure gauge in the adjusting section is 8.8 MPa of carbon dioxide supercritical, the pressure adjusting section has a residence time of about 26 seconds (calculated value), and polylactic acid is decomposed in the flat screw decompression vent section. The water pump reduced compression polymerization to restore the molecular weight of polylactic acid. It was clear that the pellets obtained were clear and dispersible to the nano level despite the starch content.

Example 3

In this example, the multistage gear type foam injection molding 'extruder shown in Fig. 7 was used with the number of multistage gears changed to 10 stages. A single screw flat screw with a diameter of 50 mm and a length of 750 mm at the bottom of the raw material supply was used. Describe the dimensions of the main part. Only the tooth thickness of the A-axis and B-axis is described, the tooth thickness of the C-axis is described, and the lower stage is the structure described as the step-down part X or the step-up part Y, and there is a description of the tooth thickness of the C-axis The stage has the structure shown as the kneading part Z. The pressure described below is the outlet pressure of the listed stage and corresponds to the inlet side of the next stage, and the unit is (MPa).

The pitch circle diameter of all gears is 46mm and module 2 is adopted.

1st stage A-axis, B-axis tooth thickness l2mm 0.74 (measured value)

2nd stage A-axis, B-axis tooth thickness 92mm 5. 19 (design value)

3-stage A-axis, B-axis tooth thickness 44 mm ZC-axis tooth thickness 18 mm 9.8 (design value)

4-stage A-axis, B-axis tooth thickness 36 mm ZC-axis tooth thickness 18 mm 9.8 (design value)

5-stage A-axis, B-axis tooth thickness l8mm 9.8 (design value)

6-stage A-axis, B-axis tooth thickness 36 mm ZC-axis tooth thickness 18 mm 9.8 (measured value)

7-stage A-axis, B-axis tooth thickness l8mm 5. 88 (design value)

8 steps A-axis, B-axis tooth thickness 22mm 2. 94 (design value)

9th stage A-axis, B-axis tooth thickness 32mm 0.2 (design value)

10th stage A-axis, B-axis tooth thickness 312mm

A water-cooled round die with an effective total length of 1200 mm was attached to the rear of the 10th stage of the multi-stage gear group. The inner diameter of the outer water-cooled round die is 80mm outlet diameter, the core water-cooled round die adopts a tapered taper, and the outer diameter is 60mm outlet diameter.

The heater temperature was set to 160 ° C, the shaft rotation speed was 80 rpm, 99.5 wt% of the main raw material polyethylene and 0.5 wt% of wax were dry blended, and the hopper force was also added. In the gas inlet Compressed air from the compressor was reduced to 0.74 (MPa) by a pressure reducing valve and injected. As a result, a cylindrical continuous foam having an outer diameter of 80 mm and an inner diameter of 60 mm was obtained. The foam cell had a small foaming ratio of about 50 times, and the time-equivalent discharge was 35 kg.

Example 4

[0047] In this example, the multistage gear type foam injection molding extruder of FIG. 7 having the same gear as in Example 3 and having 10 stages was used. However, the round die of the apparatus of Example 3 was removed, and a mechanical nozzle for an injection molding machine was attached and used. For a simple prototype test, aluminum was used for the mold, 6mm diameter holes for material leakage were provided at 8 locations, and the structure was configured to press the mechanical nozzle with hooks. In addition, a drain was installed between the mechanical nozzle and the mold, and a switching valve was installed between the direction in which the mold flows in and the direction in which the drain force flows out. The gas inlet was connected to a pressure-reducing valve of carbon dioxide and bomb that was reduced to 0.74 (MPa).

[0048] 99% by weight of the dried polylactic acid and 1% by weight of trimellitic anhydride were dry blended and supplied from the hopper at a rate of 35 kgZ, and the carbon dioxide injection loca was also supplied with carbon dioxide of 0.774 MPa. 230 ° C, 6th stage rear pressure 9.8 KMP under continuous supercritical carbon dioxide conditions After injection into the mold, the mold was water cooled. The foamed polylactic acid Toro box expanded approximately 50 times, produced fine foam nuclei, and was able to mold a Toro box with no flash marks.

Claims

The scope of the claims

[1] A processing device for continuously kneading and compressing a gas-mixed substance to process it as a fluid in a critical state, and has two or more gear-type transfer units with different transfer unit capacities. A multi-stage characterized by controlling the pressure to compress the gas contained in the fluid by the difference in the transfer section capacity of the two-stage gear-type transfer section, or by making a part of the transfer fluid flow backward to make the actual transfer capacity constant. Gear type processing equipment.

[2] The multi-stage gear type machining apparatus according to claim 1, wherein a plurality of gears paired with the two-stage gear type transfer part having different continuous transfer part capacities are provided.

[3] The multi-stage gear type machining apparatus according to claim 1 or 2, wherein the gear type transfer unit is provided following the extrusion screw.

[4] A gas injection port is provided between the gear-type transfer unit, and the transfer unit capacity by the gear at the front stage of the injection port is smaller than the transfer unit capacity by the gear at the rear stage of the injection port, which enables injection of the injection loca gas. The multistage gear type carriage device according to any one of claims 1 to 3, wherein the force is one.

5. The multistage gear type machining apparatus according to any one of claims 1 to 4, wherein the gear type transfer unit generates a pressure sufficient to form a supercritical or subcritical state.

[6] The multistage gear type cache device according to any one of claims 1 to 5, wherein the multistage gear type cache device is used for gas foam molding.

[7] A processing method such as kneading, decomposition, extraction or chemical synthesis using the multistage gear type processing apparatus according to any one of claims 1 to 5.