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JP2007218588A - Method of measuring bulk density of prefoamed particles - Google Patents

Method of measuring bulk density of prefoamed particles Download PDF

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JP2007218588A
JP2007218588A JP2006035935A JP2006035935A JP2007218588A JP 2007218588 A JP2007218588 A JP 2007218588A JP 2006035935 A JP2006035935 A JP 2006035935A JP 2006035935 A JP2006035935 A JP 2006035935A JP 2007218588 A JP2007218588 A JP 2007218588A
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bulk density
expanded particles
particles
expanded
sample collection
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JP4680086B2 (en
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Jo Tsugawa
城 津川
Satoru Saito
悟 斎藤
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Kaneka Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for measuring the proper bulk density of prefoamed particles by suppressing the shrinkage of the prefoamed particles in a manufacturing method of the prefoamed particles. <P>SOLUTION: A part of the prefoamed particles, which are prefoamed by a prefoaming device and fed to a prefoamed particle storage tank from the prefoaming device, is sampled by a sampling container through sampling piping and sampled prefoamed particles are discharged to a dryer from the sampling container by a flower to be dried by air streams while the bulk density of the dried prefoamed particles is subsequently automatically measured by a bulk density measuring instrument. After the prefoamed particles are sampled by the sampling container to be held in the sampling container for a definite time, they are discharged to the dryer. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、予備発泡装置で発泡させる発泡性熱可塑性樹脂の予備発泡粒子の嵩密度を自動的に測定するための方法に関する。   The present invention relates to a method for automatically measuring the bulk density of pre-expanded particles of a foamable thermoplastic resin to be foamed with a pre-foaming device.

発泡性熱可塑性樹脂から発泡樹脂製品を製造するには、まず原料となる熱可塑性樹脂粒子(原料樹脂)を予備発泡装置により所定の嵩密度まで発泡させ、これを成形機でさらに発泡させて成形体を成形している。この発泡樹脂製品の製造においては、前記の予備発泡粒子の嵩密度を一定にすることが、成形機に供給される予備発泡粒子の量を安定化させ、成形体の品質を安定化させるために重要である。   In order to produce a foamed resin product from a foamable thermoplastic resin, first, the thermoplastic resin particles (raw material resin) as a raw material are foamed to a predetermined bulk density by a pre-foaming device, and further foamed by a molding machine to be molded. The body is molded. In the production of the foamed resin product, to keep the bulk density of the prefoamed particles constant in order to stabilize the amount of the prefoamed particles supplied to the molding machine and to stabilize the quality of the molded body. is important.

一般的に、前記の予備発泡粒子を製造する工程としては、熱可塑性樹脂からなる一定量の原料樹脂粒子を、予備発泡加圧容器に水、分散剤、必要に応じて界面活性剤等の分散助剤とともに投入し、発泡剤を投入するとともに前記加圧容器内を所定の圧力に調整し、該加圧容器に取り付けられたジャケットに蒸気を通して加圧容器内の混合物を所定の温度に調整し、所定の温度と圧力に到達すれば、加圧容器払い出しバルブを開いて加圧容器からノズルを通して分散剤等を含んだ水と共に樹脂粒子を排出することで発泡させ、予備発泡粒子を得る。このようにして得られた予備発泡粒子は分離器で水と分離され、予備発泡粒子貯槽に送られる。   In general, the step of producing the above pre-foamed particles is to disperse a certain amount of raw material resin particles made of a thermoplastic resin into a pre-foamed pressurized container, such as water, a dispersant, and if necessary a surfactant. It is charged with an auxiliary agent, a foaming agent is charged, the inside of the pressurized container is adjusted to a predetermined pressure, and steam is passed through a jacket attached to the pressurized container to adjust the mixture in the pressurized container to a predetermined temperature. When the predetermined temperature and pressure are reached, the pressurized container discharge valve is opened, and the resin particles are discharged from the pressurized container through the nozzle together with water containing the dispersant and the like to cause foaming to obtain pre-expanded particles. The pre-expanded particles thus obtained are separated from water by a separator and sent to a pre-expanded particle storage tank.

従来より、前記予備発泡粒子の嵩密度を調整する方法としては、予備発泡中の粒子を採取し、その嵩密度を測定し、目標値との乖離をもとに予備発泡装置の運転条件(例えば、予備発泡加圧容器への原料粒子の供給量、予備発泡加圧容器の圧力、温度等)を変更することが行われている。前記予備発泡粒子の嵩密度は、前記予備発泡装置で予備発泡後の水蒸気や水に濡れている予備発泡粒子を脱水し、これを嵩密度測定装置で測定する。例えば、特許文献1には、予備発泡装置で予備発泡され該予備発泡装置から予備発泡粒子貯槽へ送られる予備発泡粒子の一部を、サンプル採取配管を介してサンプル採取容器に採取し、その後、該予備発泡粒子を送風機により前記サンプル採取容器から乾燥機に排出して予備発泡粒子を気流乾燥し、引き続き乾燥した予備発泡粒子の嵩密度を嵩密度測定機により自動的に測定し、この予備発泡粒子の嵩密度の測定結果をもとに、発泡時間の間に発泡条件を調整し、嵩密度がそろった、即ち発泡倍率が安定した予備発泡粒子を製造する方法が知られている
WO2005/87475号公報
Conventionally, as a method of adjusting the bulk density of the pre-foamed particles, the pre-foamed particles are collected, the bulk density is measured, and the pre-foaming device operating conditions (for example, based on the deviation from the target value) The amount of raw material particles supplied to the pre-foamed pressurized container, the pressure of the pre-foamed pressurized container, the temperature, etc.) are changed. The bulk density of the pre-expanded particles is determined by dehydrating the pre-foamed particles wetted with water vapor or water after pre-foaming with the pre-foaming apparatus, and measuring this with a bulk density measuring apparatus. For example, in Patent Document 1, a part of the pre-foamed particles pre-foamed by the pre-foaming device and sent from the pre-foaming device to the pre-foamed particle storage tank is collected in a sample collection container through the sample collection pipe, The pre-expanded particles are discharged from the sampling container to the dryer by a blower, the pre-expanded particles are air-dried, and then the bulk density of the dried pre-expanded particles is automatically measured by a bulk density measuring machine. Based on the measurement results of the bulk density of the particles, a method is known in which the foaming conditions are adjusted during the foaming time to produce pre-foamed particles having a uniform bulk density, that is, a stable foaming ratio.
WO2005 / 87475

前記従来公知の予備発泡粒子の自動倍率測定装置ならびに方法においては、室温、大気圧で液状を呈する発泡剤を使用する場合、工程から該予備発泡粒子を採取し、ただちに乾燥させると該予備発泡粒子が収縮すると言う課題がある。   In the conventional well-known automatic magnification measuring apparatus and method for pre-expanded particles, when using a foaming agent that exhibits a liquid state at room temperature and atmospheric pressure, the pre-expanded particles are collected by collecting the pre-expanded particles from the process and drying them immediately. There is a problem of shrinking.

これは、乾燥工程において該予備発泡粒子の表面の水分が蒸発し、その蒸発潜熱で表面が冷却され、予備発泡粒子中の気泡が収縮するためと考えられる。この収縮が起こると、実際に工程で製造される該予備発泡粒子と、自動測定で採取した該予備発泡粒子の嵩密度に相関が無くなり、予備発泡粒子の製造中に正しい嵩密度が測定できなくなるという問題がある。   This is presumably because the moisture on the surface of the pre-expanded particles evaporates in the drying step, the surface is cooled by the latent heat of evaporation, and the bubbles in the pre-expanded particles contract. When this shrinkage occurs, there is no correlation between the bulk density of the pre-foamed particles actually produced in the process and the pre-foamed particles collected by automatic measurement, and the correct bulk density cannot be measured during the production of the pre-foamed particles. There is a problem.

従って、本発明が解決しようとする課題は、例えば、水などの、室温、大気圧で液状を呈する発泡剤を使用した予備発泡粒子の製造工程において、予備発泡粒子の収縮を抑制し、適切な予備発泡粒子の嵩密度を測定することにあり、更には得られた予備発泡粒子の嵩密度の測定結果をもとに、発泡時間の間に発泡条件を調整し、嵩密度がそろった、即ち発泡倍率が安定した予備発泡粒子を製造することである。   Therefore, the problem to be solved by the present invention is to prevent the shrinkage of the pre-foamed particles in the production process of the pre-foamed particles using a foaming agent that exhibits a liquid state at room temperature and atmospheric pressure, such as water. It is to measure the bulk density of the pre-foamed particles, and further, based on the measurement result of the bulk density of the obtained pre-foamed particles, the foaming conditions are adjusted during the foaming time, This is to produce pre-expanded particles having a stable expansion ratio.

上記目的を達成するために、本発明にかかる予備発泡粒子の嵩密度の測定方法は、予備発泡装置で予備発泡され該予備発泡装置から予備発泡粒子貯槽へ送られる発泡性熱可塑性樹脂の予備発泡粒子の一部を、サンプル採取配管を介してサンプル採取容器に採取し、該予備発泡粒子を送風機により前記サンプル採取容器から乾燥機に排出して予備発泡粒子を気流乾燥し、引き続き乾燥した予備発泡粒子の嵩密度を嵩密度測定機により自動的に測定する方法において、予備発泡粒子をサンプル採取容器に採取後一定時間保持した後に乾燥機に排出することで、前記課題を解決できることを見出し本発明の完成に至った。   In order to achieve the above object, the method for measuring the bulk density of pre-expanded particles according to the present invention is a pre-expansion of a foamable thermoplastic resin pre-foamed by a pre-foaming device and sent from the pre-foaming device to a pre-foamed particle storage tank. Part of the particles are collected in a sample collection container through a sample collection pipe, and the pre-foamed particles are discharged from the sample collection container to the dryer by a blower, and the pre-foamed particles are air-dried, and then dried pre-foam. In the method of automatically measuring the bulk density of particles with a bulk density measuring device, the present invention has found that the above-mentioned problems can be solved by pre-expanded particles being collected in a sample collection container and then discharged to a dryer after being held for a certain period of time. It was completed.

即ち本発明の第1は、予備発泡粒子の嵩密度を測定する方法であって、予備発泡装置で予備発泡され該予備発泡装置から予備発泡粒子貯槽へ送られる予備発泡粒子の一部を、サンプル採取配管を介してサンプル採取容器に採取し、採取した予備発泡粒子を送風機により前記サンプル採取容器から乾燥機に排出して予備発泡粒子を気流乾燥したのち、乾燥した予備発泡粒子の嵩密度を嵩密度測定機により自動的に測定する方法において、予備発泡粒子をサンプル採取容器に採取した後、一定時間サンプル採取容器内に予備発泡粒子を保持した後、乾燥機に排出することを特徴とする予備発泡粒子の嵩密度を自動的に測定する方法に関する。   That is, the first of the present invention is a method for measuring the bulk density of pre-expanded particles, in which a part of the pre-expanded particles that are pre-expanded by the pre-expanding device and sent from the pre-expanding device to the pre-expanded particle storage tank are sampled. After collecting the pre-expanded particles collected in a sample-collecting container through a sampling pipe, discharging the pre-expanded particles from the sample-collecting container to the dryer by a blower and air-drying the pre-expanded particles, the bulk density of the dried pre-expanded particles is increased. In the method of automatically measuring by a density measuring machine, after pre-expanded particles are collected in a sample collection container, the pre-expanded particles are held in the sample collection container for a certain period of time and then discharged to a dryer. The present invention relates to a method for automatically measuring the bulk density of expanded particles.

本発明の第2は、予備発泡装置から予備発泡粒子を連続的に排出しながら、前記排出された予備発泡粒子の嵩密度を前記記載の方法により測定し、該測定結果を嵩密度比較演算装置にて目標値と比較して、その結果を予備発泡装置にフィードバックすることで、予備発泡装置で予備発泡させている予備発泡粒子の発泡条件を調整することを特徴とする予備発泡粒子の製造方法に関する。好ましい実施態様としては、前記嵩密度比較演算装置からのフィードバックにより予備発泡装置の設定圧力を調整する前記記載の製造方法に関する。   The second aspect of the present invention is to measure the bulk density of the discharged pre-expanded particles by the above-described method while continuously discharging the pre-expanded particles from the pre-expanding device, and to calculate the measurement result as a bulk density comparison calculation device. The method for producing pre-foamed particles is characterized by adjusting the foaming conditions of the pre-foamed particles pre-foamed by the pre-foaming device by feeding back the result to the pre-foaming device in comparison with the target value About. As a preferred embodiment, the present invention relates to the manufacturing method described above, wherein the set pressure of the pre-foaming device is adjusted by feedback from the bulk density comparison calculation device.

本発明に係る予備発泡粒子の嵩密度測定方法によれば、室温、大気圧で液状である発泡剤を使用した予備発泡粒子の製造の場合にも、予備発泡装置から採取した予備発泡粒子の収縮を抑制しながら、短時間で精度の良い嵩密度測定が可能になる。また、前記嵩密度の測定結果を予備発泡装置の運転条件にフィードバックすることで、所定の嵩密度の予備発泡粒子の製造が可能になる。   According to the method for measuring the bulk density of pre-expanded particles according to the present invention, the shrinkage of the pre-expanded particles collected from the pre-expanding apparatus is also used in the production of pre-expanded particles using a foaming agent that is liquid at room temperature and atmospheric pressure. It is possible to measure the bulk density with high accuracy in a short time while suppressing the above. Further, by feeding back the measurement result of the bulk density to the operating conditions of the pre-foaming apparatus, it is possible to produce pre-foamed particles having a predetermined bulk density.

以下、本発明を図1に基づいて説明する。図1は予備発泡装置10に自動嵩密度測定装置20を接続した予備発泡粒子製造装置全体を模式的に示したものである。   Hereinafter, the present invention will be described with reference to FIG. FIG. 1 schematically shows an entire pre-expanded particle manufacturing apparatus in which an automatic bulk density measuring apparatus 20 is connected to a pre-expanding apparatus 10.

予備発泡装置10は、従来から知られている方法により予備発泡粒子を得るための装置の一例であり、例えば、予備発泡加圧容器1、ノズル5、分離器6を備えている。予備発泡加圧容器1は投入口2、圧力設定器3、加圧容器払い出しバルブ4を備えている。分離器6は排水ポンプ7を備えている。   The pre-foaming apparatus 10 is an example of an apparatus for obtaining pre-foamed particles by a conventionally known method. For example, the pre-foaming apparatus 10 includes a pre-foaming pressurized container 1, a nozzle 5, and a separator 6. The pre-foamed pressurized container 1 includes an input port 2, a pressure setting device 3, and a pressurized container discharge valve 4. The separator 6 includes a drain pump 7.

予備発泡装置10により予備発泡粒子を製造する工程は以下の通りである。まず、熱可塑性樹脂粒子(以下、原料粒子と称する場合もある)、水、分散剤、必要に応じて界面活性剤等の分散助剤を予備発泡加圧容器1に投入する。次いで、予備発泡加圧容器1を加熱して予備発泡加圧容器1内の混合物を所定の温度に調整し、圧力設定器3を通じて予備発泡加圧容器1内の圧力を所定の圧力に調整する。こうして原料粒子に発泡剤を含浸させたのち、加圧容器払い出しバルブ4を開いて、ノズル5を通して低圧雰囲気下に放出する方法(除圧発泡法)により、原料粒子を発泡させて予備発泡粒子が得られる。   The process of producing the pre-foamed particles by the pre-foaming apparatus 10 is as follows. First, thermoplastic resin particles (hereinafter sometimes referred to as raw material particles), water, a dispersant, and, if necessary, a dispersion aid such as a surfactant are charged into the pre-foamed pressure vessel 1. Next, the pre-foaming pressure vessel 1 is heated to adjust the mixture in the pre-foaming pressure vessel 1 to a predetermined temperature, and the pressure in the pre-foaming pressure vessel 1 is adjusted to a predetermined pressure through the pressure setting device 3. . In this way, after the raw material particles are impregnated with the foaming agent, the pressure vessel discharge valve 4 is opened, and the raw material particles are expanded by the method of releasing into the low-pressure atmosphere through the nozzle 5 (depressurization foaming method). can get.

ここで熱可塑性樹脂粒子は、特に限定はなく、予備発泡粒子を製造するための公知の原料樹脂を使用することが出来る。例えば、ポリエチレン、ポリプロピレンなどのポリオレフィン系樹脂、ポリスチレンなどのポリスチレン系樹脂などが挙げられる。また必要に応じて、例えば、タルク等のセル造核剤をはじめ紫外線吸収剤、酸化防止剤、帯電防止剤、熱安定剤、難燃剤、着色剤、充填剤、滑剤、結晶核剤などの添加剤がブレンドされていてもよい。   Here, the thermoplastic resin particles are not particularly limited, and a known raw material resin for producing the pre-foamed particles can be used. Examples thereof include polyolefin resins such as polyethylene and polypropylene, and polystyrene resins such as polystyrene. If necessary, for example, cell nucleating agents such as talc, UV absorbers, antioxidants, antistatic agents, heat stabilizers, flame retardants, colorants, fillers, lubricants, crystal nucleating agents, etc. Agents may be blended.

ここで分散剤は、特に限定はなく、予備発泡粒子を製造するための公知の分散剤を使用することが出来る。例えば、第三リン酸カルシウム、塩基性炭酸マグネシウム、塩基性炭酸亜鉛、炭酸カルシウムなどの無機塩やベントナイト、カオリンなどの粘土類が挙げられる。   Here, the dispersant is not particularly limited, and a known dispersant for producing pre-foamed particles can be used. Examples thereof include inorganic salts such as tricalcium phosphate, basic magnesium carbonate, basic zinc carbonate, and calcium carbonate, and clays such as bentonite and kaolin.

ここで分散助剤は、特に限定はなく、予備発泡粒子を製造するための公知の分散助剤を使用することが出来る。例えば、ドデシルベンゼンスルフォン酸ソーダ、n−パラフィンスルフォン酸ソーダ、高級アルコール硫酸ソーダ、アルキルナフタレンスルフォン酸ソーダなどのアニオン性界面活性剤、塩化ベンザルコニウム、塩化アルキルトリメチルアンモニウム、塩化ジアルキルジメチルアンモニウムなどのカチオン性界面活性剤が挙げられる。   Here, the dispersion aid is not particularly limited, and a known dispersion aid for producing pre-expanded particles can be used. For example, anionic surfactants such as sodium dodecylbenzene sulfonate, sodium n-paraffin sulfonate, higher alcohol sodium sulfate, sodium alkylnaphthalene sulfonate, cations such as benzalkonium chloride, alkyltrimethylammonium chloride, dialkyldimethylammonium chloride Surfactants.

本発明においては発泡剤としては、特に限定はなく、揮発性発泡剤や無機ガス、水など、公知のものを使用することが出来るが、発泡剤が特に、室温、大気圧で液状のものである場合、例えば、ヘキサン、ヘプタン、オクタンなどの脂肪族炭化水素類、シクロペンタン、シクロヘキサン、シクロヘプタン、シクロオクタンなどの脂環式炭化水素類、トリクロロフルオロエタン、ジクロロペンタフルオロプロパンなどのハロゲン化炭化水素類、水などの場合に、本発明の方法が好適に使用出来、更には水を発泡剤と使用する場合が好ましい。   In the present invention, the foaming agent is not particularly limited, and known ones such as a volatile foaming agent, an inorganic gas, and water can be used, but the foaming agent is particularly liquid at room temperature and atmospheric pressure. In some cases, for example, aliphatic hydrocarbons such as hexane, heptane and octane, cycloaliphatic hydrocarbons such as cyclopentane, cyclohexane, cycloheptane and cyclooctane, halogenated carbons such as trichlorofluoroethane and dichloropentafluoropropane In the case of hydrogen, water, etc., the method of the present invention can be suitably used, and further, water is preferably used as a blowing agent.

このようにして得られた予備発泡粒子は分離器6で分散剤等を含んだ水と分離される。予備発泡粒子は分離器6と予備発泡粒子貯槽30をつなぐ配管8を通って予備発泡粒子貯槽30に送られる。   The pre-expanded particles thus obtained are separated from the water containing the dispersant and the like by the separator 6. The pre-expanded particles are sent to the pre-expanded particle storage tank 30 through the pipe 8 connecting the separator 6 and the pre-expanded particle storage tank 30.

本発明の自動嵩密度測定装置20は、分離器6と予備発泡粒子貯槽30をつなぐ配管8の途中から分岐して設けた、予備発泡粒子をサンプリングするためのサンプル採取配管9と、一端が該予備発泡粒子を透過させない構造を有する一定容積のサンプル採取容器12と、乾燥機15とを備え、これらが、三方弁11に接続されている。サンプル採取容器12は、加熱機14を備えた送風機13を備えている。乾燥機15は、嵩密度比較演算装置17を備えた嵩密度測定機16に接続されている。   The automatic bulk density measuring device 20 of the present invention is provided with a sample collecting pipe 9 for sampling pre-foamed particles, which is branched from the middle of a pipe 8 connecting the separator 6 and the pre-foamed particle storage tank 30, and one end of the pipe A fixed-volume sample collection container 12 having a structure that does not allow the pre-expanded particles to pass therethrough and a dryer 15 are provided, and these are connected to the three-way valve 11. The sample collection container 12 includes a blower 13 including a heater 14. The dryer 15 is connected to a bulk density measuring machine 16 provided with a bulk density comparison calculation device 17.

自動嵩密度測定装置20による予備発泡粒子の測定は、以下のようにして行われる。予備発泡中に、三方弁11によりサンプル採取配管9とサンプル採取容器12とを連通させ、サンプル採取配管9と乾燥機15とは遮断して、分離器6と予備発泡粒子貯槽30の間の配管8から予備発泡粒子をサンプル採取配管9を通じ、三方弁11を経由してサンプル採取容器12に採取する。   The measurement of the pre-expanded particles by the automatic bulk density measuring device 20 is performed as follows. During the pre-foaming, the three-way valve 11 causes the sample collecting pipe 9 and the sample collecting container 12 to communicate with each other, the sample collecting pipe 9 and the dryer 15 are disconnected, and the pipe between the separator 6 and the pre-foamed particle storage tank 30. The pre-expanded particles are collected from the sample collection pipe 12 through the sample collection pipe 9 and the three-way valve 11.

三方弁11は、一般に用いられる三方ボール弁を用いることが出来る。市販されている三方ボール弁には、Lポート式とTポート式の2種類があるが、本発明ではLポート式を用いることが好ましい。これは、3方向の流体の方向転換を行なうためのボール弁で、L字型の流路を備えたボールを90度回転させることによって、2方弁を3個使用する代わりに3方弁なら1個で方向切り替えできるものである。三方弁の口径は、予備発泡粒子が閉塞しない大きさがあればよく、予備発泡粒子の直径が2mm程度であれば、10A(内径およそ10mm)以上、予備発泡粒子の直径が10mm程度であれば、50A(内径およそ50mm)以上で、閉塞することなく採取できる。三方ボール弁には、ボール部分の径が配管の径より小さいタイプと、両者が同じ径(フルボアと称される)ものがある。予備発泡粒子が閉塞しない限り、どちらのタイプでも使用する事ができる。   The three-way valve 11 can be a commonly used three-way ball valve. There are two types of commercially available three-way ball valves, an L port type and a T port type. In the present invention, it is preferable to use an L port type. This is a ball valve for changing the direction of fluid in three directions. By rotating a ball with an L-shaped flow path by 90 degrees, instead of using three two-way valves, The direction can be switched by one. The diameter of the three-way valve only needs to be large enough to prevent the pre-expanded particles from being blocked. If the diameter of the pre-expanded particles is about 2 mm, the diameter of the pre-expanded particles is about 10 mm or more. , 50A (inner diameter approximately 50 mm) or more, can be collected without clogging. Three-way ball valves include a type in which the diameter of the ball portion is smaller than the diameter of the pipe, and a type in which both have the same diameter (referred to as a full bore). Either type can be used as long as the pre-expanded particles are not blocked.

サンプル採取容器12の他端側(三方弁11を接続した側と反対側)には、予備発泡粒子を透過させないためのメッシュが設けられている。メッシュは、予備発泡粒子を捕捉するが水およびガスを通過できるものであれば、線径ならびに目開きは限定されない。予備発泡装置10(予備発泡加圧容器1)の内圧により、予備発泡粒子と水ならびにガスが三方弁11を通過してサンプル採取容器12に流入し、流入した予備発泡粒子はメッシュで捕捉され、水の一部とガスはメッシュを通過し、さらに加熱機14と送風機13を逆流して外部へ放出される。このようにして、予備発泡装置10の内圧により、メッシュで仕切られたサンプル採取容器12内の空間Aに一定量の予備発泡粒子が充填される。前記予備発泡装置10の内圧が予備発泡粒子をサンプル採取容器12内に充填するのに不十分な場合には、メッシュを通してサンプル採取容器12内を減圧にすることで、サンプル採取容器12内への予備発泡粒子の充填をスムーズにすることができる。サンプル採取容器12の容量、すなわちメッシュで仕切られた空間Aの容積は、0.05〜10L、より好ましくは0.3〜3L程度である。サンプル採取容器12の容量が大きすぎると予備発泡粒子の迅速な乾燥が困難になり、発泡時間の間に嵩密度の測定と測定結果のフィードバックができない場合があり、またサンプル採取容器12の容量が小さすぎる場合には嵩密度の測定精度が低下するので、好ましくない。   On the other end side of the sample collection container 12 (the side opposite to the side where the three-way valve 11 is connected), a mesh for preventing the pre-expanded particles from passing therethrough is provided. As long as the mesh captures the pre-expanded particles but can pass water and gas, the wire diameter and the mesh are not limited. Due to the internal pressure of the pre-foaming device 10 (pre-foaming pressurized container 1), the pre-foamed particles, water and gas pass through the three-way valve 11 and flow into the sample collection container 12, and the pre-foamed particles that flow in are captured by the mesh, Part of the water and gas pass through the mesh, and then flow backward through the heater 14 and the blower 13 and are discharged to the outside. In this way, the space A in the sample collection container 12 partitioned by the mesh is filled with a certain amount of pre-expanded particles by the internal pressure of the pre-expanding device 10. When the internal pressure of the pre-foaming device 10 is insufficient to fill the pre-expanded particles into the sample collection container 12, the pressure inside the sample collection container 12 is reduced through the mesh to The pre-expanded particles can be filled smoothly. The capacity of the sample collection container 12, that is, the volume of the space A partitioned by the mesh is about 0.05 to 10L, more preferably about 0.3 to 3L. If the capacity of the sample collection container 12 is too large, it becomes difficult to quickly dry the pre-expanded particles, and the bulk density may not be measured during the foaming time and the measurement results may not be fed back. If it is too small, the measurement accuracy of the bulk density decreases, which is not preferable.

次に、三方弁11を切り替えて、サンプル採取配管9とサンプル採取容器12とを遮断した後、採取された予備発泡粒子は、次工程の乾燥における収縮を抑制する目的で、一定時間、そのまま保持される。   Next, after switching the three-way valve 11 to shut off the sample collection pipe 9 and the sample collection container 12, the collected pre-expanded particles are held as they are for a certain period of time for the purpose of suppressing shrinkage during drying in the next step. Is done.

前記の一定時間とは、サンプル採取配管9とサンプル採取容器12とを遮断する時点を開始時とし、後述の、予備発泡粒子を乾燥機15に送るために送風機13で気流を発生させる時点を終了時とする。   The predetermined time is the time when the sample collection pipe 9 and the sample collection container 12 are shut off, and the time when the air flow is generated by the blower 13 to send the pre-expanded particles to the dryer 15, which will be described later, is ended. It is time.

保持される時間の長さは、予備発泡粒子の温度、樹脂組成、発泡剤(ガス)の沸点にもよるが、発泡剤が水の場合、0.5分間以上とすることが好ましく、さらには1分間以上とすることがより好ましい。収縮抑制の目的からは、この保持時間は長いほうが好ましい。一方、この測定結果をフィードバックするためには、この保持時間を長くすると、応答が遅れて目的とする嵩密度の予備発泡粒子が得られなく恐れがあるため、5分以下が好ましく、更に好ましくは3分以下である。   The length of time to be retained depends on the temperature of the pre-foamed particles, the resin composition, and the boiling point of the foaming agent (gas), but when the foaming agent is water, it is preferably 0.5 minutes or more, More preferably, it is 1 minute or longer. For the purpose of suppressing shrinkage, it is preferable that this holding time is long. On the other hand, in order to feed back the measurement result, if this holding time is lengthened, the response may be delayed, and the pre-expanded particles having the desired bulk density may not be obtained. 3 minutes or less.

サンプル採取容器12に採取された直後の予備発泡粒子の内部にはガス化した発泡剤が含まれている。WO2005/87475号公報に記載の方法によって、採取直後の予備発泡粒子をただちに乾燥した場合には、表面の水分が蒸発する際に蒸発潜熱によって予備発泡粒子の表面が冷却され、そのために内部の発泡剤が液化して予備発泡粒子の内部が減圧になり、予備発泡粒子を形成する気泡構造が潰れて収縮する。一方、前述のように予備発泡粒子を一定時間保持すると、その間に予備発泡粒子の内部には、徐々に周辺の空気が入り込むので、その後に乾燥する際に予備発泡粒子の内部の減圧度は低くなり、収縮が抑制されるものと考えられる。   The pre-expanded particles immediately after being collected in the sample collection container 12 contain a gasified foaming agent. When the pre-expanded particles immediately after collection are immediately dried by the method described in WO 2005/87475, the surface of the pre-expanded particles is cooled by latent heat of evaporation when the water on the surface evaporates. The agent is liquefied and the inside of the pre-expanded particles is depressurized, and the cell structure forming the pre-expanded particles is crushed and contracted. On the other hand, if the pre-expanded particles are held for a certain period of time as described above, the surrounding air gradually enters the pre-expanded particles during that time, so the degree of vacuum inside the pre-expanded particles is low when drying thereafter. Therefore, it is considered that shrinkage is suppressed.

この様に一定時間サンプル採取容器に保持された予備発泡粒子は、次に、送風機13で発生させた気流で押し出し、乾燥機15に送るとともに、脱水乾燥させる。   The pre-expanded particles thus held in the sample collection container for a certain period of time are then pushed out by the air flow generated by the blower 13 and sent to the dryer 15 and dehydrated and dried.

前記の気流は、乾燥に要する時間を短くするために加熱機14を通して加熱しても良い。該加熱機14は、一般的に用いられる空気加熱ヒータを用いることができる。加熱機14の例としては、シェル型ヒータ、ダクトヒータ、ねじ込みヒータなどが挙げられ、予備発泡粒子をサンプル採取容器12から乾燥機15へ送り、脱水乾燥させるのに必要とする風量と温度に応じて適当な方式と能力のものを選択すればよい。乾燥に使用する送風機13からの風量および加熱機14で調整される乾燥空気の温度は、予備発泡粒子の表面の水分量、乾燥空気の湿度、予備発泡粒子の樹脂組成、発泡剤の種類や量等に応じて設定すればよい。乾燥温度が低いと乾燥時間が長くなるので、この場合は送風機13からの風量を増すとよい。   The airflow may be heated through the heater 14 in order to shorten the time required for drying. The heater 14 can be a commonly used air heater. Examples of the heater 14 include a shell-type heater, a duct heater, a screw heater, and the like. Depending on the air volume and temperature required to send the pre-foamed particles from the sample collection container 12 to the dryer 15 for dehydration and drying. Select the one with the appropriate method and ability. The amount of air from the blower 13 used for drying and the temperature of the drying air adjusted by the heater 14 are the moisture content on the surface of the pre-foamed particles, the humidity of the dry air, the resin composition of the pre-foamed particles, and the type and amount of the foaming agent. What is necessary is just to set according to etc. Since drying time will become long if drying temperature is low, it is good to increase the air volume from the air blower 13 in this case.

前記の乾燥機15は、一般的に粉粒体の乾燥に用いられる方式の乾燥機を用いることができる。乾燥機15での予備発泡粒子の滞留時間は、乾燥に必要な時間をとればよい。乾燥速度が速く、予備発泡粒子がサンプル採取容器12から乾燥機15にいたるまでの数秒で乾燥する場合には、気流乾燥あるいはフラッシュ乾燥と呼ばれる乾燥機を用いることができる。乾燥速度が遅い場合は、サイクロン乾燥機や流動層乾燥機などを用いることができる。乾燥機15を、サイクロン乾燥機のような、内部で乾燥空気と予備発泡粒子が回転するような構造にしておけば、送風している限り乾燥機内で予備発泡粒子が滞留し、乾燥が完了するまで必要な滞留時間を自在に確保することができる。ただし、過度に乾燥させると、表面に水分の無くなった予備発泡粒子は乾燥機15内部で帯電し、後述の嵩密度測定時に粒子同士が反発して、正しい嵩密度を測定できない場合がある。この場合、乾燥までに、予備発泡粒子に帯電防止剤を添加(噴霧)し、装置をアースしておくこと等により、正常に嵩密度を測定できる。帯電防止剤は、市販の帯電防止剤、界面活性剤等を使用する事ができる。乾燥粒子の帯電対策としては、乾燥に用いる空気を加湿しておくことも効果的である。   As the dryer 15, a dryer of a system generally used for drying powder particles can be used. The residence time of the pre-expanded particles in the dryer 15 may be a time required for drying. When the drying speed is fast and the pre-expanded particles are dried in a few seconds from the sample collection container 12 to the dryer 15, a dryer called air flow drying or flash drying can be used. When the drying speed is low, a cyclone dryer or a fluidized bed dryer can be used. If the dryer 15 has a structure in which dry air and pre-expanded particles rotate inside, such as a cyclone dryer, the pre-expanded particles stay in the dryer as long as the air is blown, and the drying is completed. The necessary residence time can be secured freely. However, when excessively dried, the pre-expanded particles whose surface has no moisture are charged inside the dryer 15 and the particles repel at the time of measuring the bulk density described later, so that the correct bulk density may not be measured. In this case, the bulk density can be measured normally by adding (spraying) an antistatic agent to the pre-expanded particles and grounding the device before drying. As the antistatic agent, commercially available antistatic agents, surfactants and the like can be used. As a countermeasure against electrification of dry particles, it is also effective to humidify the air used for drying.

乾燥した予備発泡粒子は、乾燥機15底部の払い出しバルブ18から嵩密度測定機16に投入される。嵩密度測定機16は、一定体積の容器にサンプルを採取し、このサンプルの重量を測定することで、嵩密度が計算できるようになっている。また、嵩密度測定機16は、測定の済んだサンプルを外部に排出する機構を備えている。嵩密度の測定結果は、嵩密度比較演算装置17で演算される。嵩密度比較演算装置17は、嵩密度測定機16から出力された嵩密度の測定結果の電気信号を、パソコンあるいはプログラマブルコントローラなどに入力して、目標値と比較演算する。嵩密度比較演算装置17で演算され、目標の嵩密度と異なっている場合は、予備発泡装置10の圧力設定器3に新たな圧力設定値を設定する信号が送られる。嵩密度測定機16および嵩密度比較演算装置17は公知のものを用いることができる。   The dried pre-expanded particles are put into the bulk density measuring device 16 from the discharge valve 18 at the bottom of the dryer 15. The bulk density measuring device 16 can calculate the bulk density by collecting a sample in a container having a constant volume and measuring the weight of the sample. Further, the bulk density measuring device 16 includes a mechanism for discharging the measured sample to the outside. The measurement result of the bulk density is calculated by the bulk density comparison calculation device 17. The bulk density comparison calculation device 17 inputs the electrical signal of the measurement result of the bulk density output from the bulk density measuring device 16 into a personal computer or a programmable controller, and compares it with the target value. When it is calculated by the bulk density comparison calculation device 17 and is different from the target bulk density, a signal for setting a new pressure set value is sent to the pressure setting device 3 of the preliminary foaming device 10. Known devices can be used for the bulk density measuring device 16 and the bulk density comparison calculation device 17.

以下に実施例により本発明を更に説明するが、本発明はこの実施例に限定されるものではない。なお、以下の実施例中、「部」は「重量部」を表す。   EXAMPLES The present invention will be further described below with reference to examples, but the present invention is not limited to these examples. In the following examples, “part” represents “part by weight”.

(実施例1〜4)
ポリオレフィン系樹脂予備発泡粒子の製造に、本発明を適用した例を挙げる。ポリプロピレン系樹脂であるエチレン−プロピレンランダム共重合体(融点145℃、MI値7g/10分)100部に対し、親水性ポリマーとしてエチレン−(メタ)アクリル酸共重合体をカリウムイオン架橋したエチレン系アイオノマー樹脂(商品名ハイミランSD100 三井デュポンポリケミカル社製 )2部と、トリアジン骨格を有し単位トリアジン骨格あたりの分子量が300以下の化合物としてメラミン(商品名メラミン BASF社製)1部と、無機充填剤としてタルク(平均粒径8μm)0.15部と、着色剤としてカーボンブラック2.6部とを添加し、50mmφ単軸押出機で溶融混練した後、直径2.2mmφの円筒ダイよりストランド状に押出し、水冷後、カッターで切断し、円柱状のポリオレフィン系樹脂組成物からの樹脂粒子(ペレット)(1.8mg/粒)を得た。
(Examples 1-4)
The example which applied this invention to manufacture of polyolefin resin pre-expanded particle is given. Ethylene-propylene random copolymer (melting point 145 ° C., MI value 7 g / 10 min) 100 parts of polypropylene resin, ethylene- (meth) acrylic acid copolymer as a hydrophilic polymer crosslinked with potassium ion 2 parts of ionomer resin (trade name High Milan SD100 manufactured by Mitsui DuPont Polychemical Co., Ltd.), 1 part of melamine (trade name made by melamine BASF) as a compound having a triazine skeleton and a molecular weight per unit triazine skeleton of 300 or less, and inorganic filling Add 0.15 part of talc (average particle size 8 μm) as an agent and 2.6 parts of carbon black as a colorant, melt and knead with a 50 mmφ single screw extruder, and then form a strand from a cylindrical die with a diameter of 2.2 mmφ Extruded into water, cooled with water, cut with a cutter, from a cylindrical polyolefin resin composition To obtain resin particles (pellets) (1.8 mg / particle).

前記の得られた樹脂粒子100部(800kg)と、無機分散剤として第三リン酸カルシウム0.75部と、分散助剤としてn−パラフィンスルフォン酸ソーダ0.01部を、水200部と共に、図1に示す予備発泡装置10の予備発泡加圧容器1(容量3.0m3)に仕込んだ後、攪拌下で予備発泡加圧容器1内の温度を151℃まで加熱した。その後、圧力設定器3から圧縮空気を供給して予備発泡加圧容器1を2.3MPaまで昇圧し、該容器内温度で30分間保持した。その後、嵩密度が65〜71g/Lになるように予備発泡加圧容器1内の圧力を圧力設定器3からの圧縮空気で調節しながら、加圧容器払い出しバルブ4を開き、ノズル5(開口径3.6mmφ、開口数5穴のオリフィス)を通して、100℃の蒸気飽和雰囲気下に放出して予備発泡粒子を得た。発泡した予備発泡粒子は、分離器6で水と分離し、配管8(直径250mm)を通って、予備発泡粒子貯槽30に送った。 FIG. 1 shows 100 parts (800 kg) of the obtained resin particles, 0.75 part of tricalcium phosphate as an inorganic dispersant, 0.01 part of sodium n-paraffin sulfonate as a dispersion aid, and 200 parts of water. The pre-foaming pressure vessel 1 (capacity 3.0 m 3 ) of the pre-foaming device 10 shown in FIG. 2 was charged, and the temperature in the pre-foaming pressure vessel 1 was heated to 151 ° C. with stirring. Thereafter, compressed air was supplied from the pressure setting device 3 to raise the pressure of the pre-foamed pressurized container 1 to 2.3 MPa, and the temperature was kept at the internal temperature for 30 minutes. Thereafter, while adjusting the pressure in the pre-foamed pressurized container 1 with compressed air from the pressure setting device 3 so that the bulk density becomes 65 to 71 g / L, the pressurized container discharge valve 4 is opened and the nozzle 5 (opened) is opened. Pre-expanded particles were obtained by discharging into a steam saturated atmosphere at 100 ° C. through an orifice having a diameter of 3.6 mmφ and a numerical aperture of 5 holes. The foamed pre-expanded particles were separated from water by the separator 6 and sent to the pre-expanded particle storage tank 30 through the pipe 8 (diameter 250 mm).

このとき、前記分離器6と予備発泡粒子貯留槽30とをつなぐ配管8の途中に接続した50Aのサンプル採取配管9を通じて予備発泡粒子をサンプリングした。サンプリングした予備発泡粒子は、50Aの三方弁11がサンプル採取配管9とサンプル採取容器12に開となったときに、サンプル採取配管9および三方弁11を経て、容量1.5Lのサンプル採取容器12の空間A内に充填された。10秒後に、予備発泡粒子の充填が完了し、三方弁11を切り替えて、サンプル採取配管9とサンプル採取容器12とを遮断した。   At this time, the pre-expanded particles were sampled through the 50 A sample collection pipe 9 connected in the middle of the pipe 8 connecting the separator 6 and the pre-foamed particle storage tank 30. The sampled pre-expanded particles pass through the sample collection pipe 9 and the three-way valve 11 when the 50A three-way valve 11 is opened to the sample collection pipe 9 and the sample collection container 12, and the sample collection container 12 having a capacity of 1.5L. The space A was filled. Ten seconds later, the filling of the pre-expanded particles was completed, and the three-way valve 11 was switched to shut off the sample collection pipe 9 and the sample collection container 12.

ここで、予備発泡粒子を表1に記載の時間保持した。   Here, the pre-expanded particles were held for the time shown in Table 1.

次に送風機13から5.0m3/分、静圧4.0kPaの空気を排出し、加熱機14を空気温度が110℃になるように加熱し、三方弁11を乾燥機15とサンプル採取容器12に開とした。この空気の静圧でサンプル採取容器12に充填されていた予備発泡粒子は、三方弁11を通って、乾燥機15に送られた。送風開始後60秒で送風機13を停止し、乾燥機15底部の払い出しバルブ18を開けて、表1に示す収縮率のとおり収縮が抑制された状態で乾燥の完了した予備発泡粒子を公知の構造の嵩密度測定機16に落下、投入した。 Next, air of 5.0 m 3 / min and static pressure of 4.0 kPa is discharged from the blower 13, the heater 14 is heated so that the air temperature becomes 110 ° C., and the three-way valve 11 is connected to the dryer 15 and the sampling container. 12 was open. The pre-expanded particles filled in the sample collection container 12 with the static pressure of the air passed through the three-way valve 11 and were sent to the dryer 15. The blower 13 is stopped 60 seconds after the start of air blowing, the discharge valve 18 at the bottom of the dryer 15 is opened, and the pre-expanded particles that have been dried in a state in which the shrinkage is suppressed as shown in Table 1 are known structures. The product was dropped into the bulk density measuring machine 16 and charged.

嵩密度測定機16では、容量1.0Lの計量カップに予備発泡粒子が投入されて一定体積が採取された。余剰の予備発泡粒子0.5Lは前記計量カップから溢れて外部に排出された。前記計量カップは計量器により吊り下げられており、予備発泡粒子の重量W(g)が測定され、予備発泡粒子の嵩密度が、W/1.0=W(g/L)と求められた。次いで、測定を終えた予備発泡粒子が前記計量カップの底部に設けられた排出弁から外部に排出され、嵩密度の測定が完了した。真の嵩密度に対する誤差を表1に示す。   In the bulk density measuring device 16, the pre-expanded particles were put into a measuring cup having a capacity of 1.0 L, and a certain volume was collected. Excess pre-expanded particles 0.5 L overflowed from the measuring cup and discharged to the outside. The measuring cup was suspended by a measuring instrument, the weight W (g) of the pre-expanded particles was measured, and the bulk density of the pre-expanded particles was determined as W / 1.0 = W (g / L). . Next, the pre-expanded particles for which measurement was completed were discharged to the outside from a discharge valve provided at the bottom of the measuring cup, and the measurement of the bulk density was completed. Table 1 shows the error relative to the true bulk density.

Figure 2007218588
さらに、アナログ信号入出力端子を内蔵したパソコンからなる公知の嵩密度比較演算装置17により測定結果と目標値を比較し、設定圧力を調節する信号を圧力設定器3に送りながら、予備発泡粒子の製造を続けた。製造開始から終了までに測定した嵩密度の測定結果は、いずれも目標とする範囲である65〜71g/Lにおさまっていた。
Figure 2007218588
Further, the measurement result and the target value are compared by a known bulk density comparison arithmetic unit 17 composed of a personal computer having a built-in analog signal input / output terminal, and a signal for adjusting the set pressure is sent to the pressure setter 3, Production continued. The measurement results of the bulk density measured from the start to the end of the production were all within the target range of 65 to 71 g / L.

(比較例1)
サンプル採取容器12に採取した予備発泡粒子を所定時間保持することなく、すぐに乾燥機15に送って乾燥した以外は、実施例1と同じ装置を用いて、同様の方法により予備発泡粒子の嵩密度を測定をした。
(Comparative Example 1)
Except for holding the pre-expanded particles collected in the sample collection container 12 for a predetermined time, immediately sending them to the dryer 15 and drying them, the bulk of the pre-expanded particles was obtained by the same method using the same apparatus as in Example 1. Density was measured.

この方法だと、予備発泡粒子は著しく収縮してしまい、製造された予備発泡粒子の嵩密度と自動測定した嵩密度とに相関が無かった。   With this method, the pre-expanded particles contracted remarkably, and there was no correlation between the bulk density of the prepared pre-expanded particles and the automatically measured bulk density.

本発明の一実施形態の自動嵩密度測定装置を予備発泡装置に適用した予備発泡粒子製造装置の全体フロー図である。1 is an overall flow diagram of a pre-foamed particle manufacturing apparatus in which an automatic bulk density measuring apparatus according to an embodiment of the present invention is applied to a pre-foaming apparatus.

符号の説明Explanation of symbols

1 予備発泡加圧容器
2 投入口
3 圧力設定器
4 加圧容器払い出しバルブ
5 ノズル
6 分離器
7 排水ポンプ
8 配管
9 サンプル採取配管
10 予備発泡装置
11 三方弁
12 サンプル採取容器
13 送風機
14 加熱機
15 乾燥機
16 嵩密度測定機
17 嵩密度比較演算装置
18 乾燥機払い出しバルブ
20 自動嵩密度測定装置
30 予備発泡粒子貯槽
m メッシュ
DESCRIPTION OF SYMBOLS 1 Prefoaming pressurization container 2 Input port 3 Pressure setting device 4 Pressurization container discharge valve 5 Nozzle 6 Separator 7 Drain pump 8 Piping 9 Sample collection piping 10 Prefoaming device 11 Three-way valve 12 Sample collection container 13 Blower 14 Heater 15 Dryer 16 Bulk density measuring device 17 Bulk density comparison calculation device 18 Dryer discharge valve 20 Automatic bulk density measuring device 30 Pre-foamed particle storage tank m mesh

Claims (3)

予備発泡粒子の嵩密度を測定する方法であって、予備発泡装置で予備発泡され該予備発泡装置から予備発泡粒子貯槽へ送られる予備発泡粒子の一部を、サンプル採取配管を介してサンプル採取容器に採取し、採取した予備発泡粒子を送風機により前記サンプル採取容器から乾燥機に排出して予備発泡粒子を気流乾燥したのち、乾燥した予備発泡粒子の嵩密度を嵩密度測定機により自動的に測定する方法において、予備発泡粒子をサンプル採取容器に採取した後、一定時間サンプル採取容器内に予備発泡粒子を保持した後、乾燥機に排出することを特徴とする予備発泡粒子の嵩密度を自動的に測定する方法。   A method for measuring the bulk density of pre-expanded particles, wherein a part of the pre-expanded particles that are pre-expanded by a pre-expanding device and sent from the pre-expanding device to a pre-expanded particle storage tank is sampled through a sample collection pipe. The pre-expanded particles collected are discharged from the sample collection container to the dryer by a blower and air-dried, and the bulk density of the dried pre-expanded particles is automatically measured by a bulk density measuring machine. In this method, after pre-expanded particles are collected in a sample collection container, the pre-expanded particles are automatically retained in the sample collection container for a certain period of time and then discharged into a dryer. How to measure. 予備発泡装置から予備発泡粒子を連続的に排出しながら、前記排出された予備発泡粒子の嵩密度を請求項1に記載の方法により測定し、該測定結果を嵩密度比較演算装置にて目標値と比較して、その結果を予備発泡装置にフィードバックすることで、予備発泡装置で予備発泡させている予備発泡粒子の発泡条件を調整することを特徴とする予備発泡粒子の製造方法。   While continuously discharging the pre-expanded particles from the pre-expanding device, the bulk density of the discharged pre-expanded particles is measured by the method according to claim 1, and the measurement result is set to a target value by a bulk density comparison calculation device. The method for producing pre-expanded particles is characterized in that the foaming conditions of the pre-expanded particles preliminarily expanded by the pre-expanding device are adjusted by feeding back the result to the pre-expanding device. 前記嵩密度比較演算装置からのフィードバックにより予備発泡装置の設定圧力を調整する請求項2記載の製造方法。   The manufacturing method of Claim 2 which adjusts the setting pressure of a preliminary | backup foaming apparatus with the feedback from the said bulk density comparison calculating apparatus.
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