KR100820862B1 - Method for regeneration of releasing agent solution containing graphite - Google Patents

Method for regeneration of releasing agent solution containing graphite Download PDF

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KR100820862B1
KR100820862B1 KR1020070035689A KR20070035689A KR100820862B1 KR 100820862 B1 KR100820862 B1 KR 100820862B1 KR 1020070035689 A KR1020070035689 A KR 1020070035689A KR 20070035689 A KR20070035689 A KR 20070035689A KR 100820862 B1 KR100820862 B1 KR 100820862B1
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graphite
release agent
agent solution
waste
tea
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KR1020070035689A
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Korean (ko)
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손명관
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(주)케미텍
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00—Moulds or cores; Details thereof or accessories therefor
    • B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
    • B29C33/58—Applying the releasing agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Mold Materials And Core Materials (AREA)

Abstract

A method for regenerating a waste releasing solution containing graphite is provided to re-disperse graphite contained in the waste releasing solution, thereby recycling the waste releasing solution. A method for regenerating a waste releasing solution containing graphite is performed by adding TEA(triethylamine) into the waste releasing solution to disperse graphite condensed in the waste releasing solution again. The TEA has a content of 0.5-2.0 wt%, based on the waste releasing solution containing 15-30 wt% of graphite. Before adding the TEA into the waste releasing solution, impurities are removed from the waste releasing solution.

Description

흑연 이형제의 재생 방법{Method for regeneration of releasing agent solution containing graphite}Method for regeneration of graphite release agent {Method for regeneration of releasing agent solution containing graphite}

본 발명은 폐 흑연 이형제의 재생 방법에 관한 것이다. 보다 상세하게는 흑연을 함유한 수성 폐 이형제 용액의 재생 방법에 관한 것이다.The present invention relates to a method for regenerating waste graphite release agent. More particularly, the present invention relates to a method for regenerating an aqueous waste release agent solution containing graphite.

이형제는 두 물질의 표면 사이에서 발생하는 접착성을 제거하는 역할을 하는 물질로 고무, 플라스틱, 수지 등 공업제품의 가압성형, 사출성형 등의 가공시에 이것들의 재료가 금형 등의 모형에 접착 또는 점착하는 것을 방지하고 성형품의 인출성 향상이나 표면 미관 향상을 위하여 재료의 내부나 금형의 표면에 처리하는 화학 약제 또는 다이캐스팅 금형이나 사출 금형 내지 프레스 등의 단조 금형 등에 있어서, 금형과 성형물과의 분리를 용이하게 하고 성형물의 성형성이 좋도록 하기 위해 금형의 상형과 하형의 성형물이 접하는 내측면에 도포하는 화학약제를 일컫는다.A release agent is a substance that removes the adhesiveness generated between the surfaces of two materials, and these materials adhere to a mold or the like during press molding or injection molding of industrial products such as rubber, plastic, and resin. The separation between the mold and the molded product in a chemical agent or a forging die such as a die casting mold or an injection mold or a press to prevent sticking and to improve the drawability of the molded article or to improve the surface aesthetics. It refers to a chemical agent applied to the inner surface of the molding of the upper mold and the lower mold of the mold in order to facilitate the moldability of the molding.

이형제는 그 종류가 매우 다양하여 물리적 특징이나 화학적 구성 및 산업상의 이용 형태에 따라 그 분류방법도 여러 가지이다. 예를 들어, 응용 형태로 볼 때 오일형, emulsion형, 오일 컴파운드형 등이 있으며 사용상의 용도와 목적에 따라 다양하게 이용되고 있다. There are many different types of release agents, depending on their physical characteristics, chemical composition and industrial use. For example, in the form of application, there are oil type, emulsion type, oil compound type, etc., which are used in various ways depending on the purpose and purpose of use.

이와 같이 이형제는 형태와 원료조성은 매우 다양하나 공통적으로 이형과정의 온도에서 적어도 한쪽 표면과는 불활성이어야 하고 표면 장력이 낮아야 하며, 분자간력 및 응집력이 약하다는 특성이 필요하며 특히 낮은 표면 장력은 금형에의 웨팅(wetting)성에서 매우 중요하다. 이러한 특성 외에 빌드 업(build up)이 없어야 하고 몰드 청결성, 친화성, 형태와 시간적인 적용의 용이성, 인체에 대한 안정성, 가격 등이 이형제를 선택하는 기준이 될 수 있다. As described above, the release agent varies widely in form and raw material composition. However, at the temperature of the release process, the release agent must be inert with at least one surface and have a low surface tension, and have a low intermolecular and cohesive force. Very important in the wetting of the In addition to these properties, there should be no build up, and mold cleanliness, affinity, ease of shape and time application, stability to human body, and price may be criteria for selecting a release agent.

한편, 이형제는 유기용제에 오일을 용해한 후 금형에 방출하는 방법으로 사용되고 있는 용제형 이형제와 물로 희석하여 사용하는 수성 이형제가 있는 바, 용제형 이형제는 거기에 포함되어 있는 다량의 용제의 휘산으로 인해 환경 오염뿐 아니라 작업환경의 악화 및 화재 발생의 문제를 파생시키는 단점이 있다. 이에 따라 환경 오염을 방지하기 위한 국제적 노력의 일환으로 작업장에서 유기용제 사용이 점차 규제됨에 따라 유기용제의 독성 및 화재의 위험성이 없어 용제형 이형제를 대체할 수 있는 친환경적인 것으로 평가되는 수성 이형제가 개발되고 있으나, 희석제로 물을 사용하므로 건조성이 나쁘고 금형에 대한 젖음성이 나쁘며 유화제를 사용하기 때문에 정밀성이 떨어지는 단점이 있다. 또한, 수성 이형제는 수용액 상태로서, 운송이 어렵고 운송비가 높은 단점을 가지고 있었다.On the other hand, the release agent is a solvent-type release agent that is used as a method of dissolving oil in an organic solvent and then released to the mold and an aqueous release agent to be diluted with water, so that the solvent release agent is due to the volatilization of a large amount of solvent contained therein In addition to environmental pollution, there are disadvantages that lead to deterioration of the working environment and problems of fire. Accordingly, as the use of organic solvents is increasingly regulated in the workplace as part of international efforts to prevent environmental pollution, water-based release agents that are considered eco-friendly to replace solvent-type release agents are developed because there is no danger of toxicity and fire of organic solvents. However, since water is used as a diluent, there is a disadvantage in that the dryness is poor, the wettability to the mold is bad, and the precision is poor because an emulsifier is used. In addition, the aqueous release agent was an aqueous solution, it was difficult to transport and had a high transport cost.

이에 국내에서도 용제형 이형제의 환경오염 문제를 해결하고, 종래 수성 이형제의 단점을 보완한 수성 이형제의 개발이 요구되고 있었다.Accordingly, in Korea, it has been required to solve the problem of environmental pollution of the solvent type release agent, and to develop an aqueous release agent that supplements the disadvantages of the conventional aqueous release agent.

한편, 이형제를 금형에 도포하기 위하여 종래에는 사람이 수작업으로 이형제 를 분사하였으나, 작업 속도가 낮고, 인건비의 상승, 보건상의 문제 등으로 인해 로보트 등 자동화 장치를 사용한 이형제 분사장치가 개발되어 사용되고 있다. 그러나, 금형 및 제품의 종류에 따라 이형제의 분사 회수가 다르고 고속작동되는 사출금형에서는 이형제의 분사회수 및 분사량의 조절이 일정치 않으므로 인한 시스템의 자동화가 어렵고, 또한, 수성 이형제가 가진 젖음성, 건조성 및 정밀성 불량으로 인해 다량으로 이형제를 사용함으로 인한 제품 제작 원가 상승이 문제되고 있다.Meanwhile, in order to apply a mold release agent to a mold, a person manually sprays the mold release agent, but due to low work speed, increase in labor costs, and health problems, a mold release agent injector using an automated device such as a robot has been developed and used. However, the injection frequency of the release agent varies according to the mold and the type of the product, and in the injection mold having a high speed, it is difficult to automate the system due to the inability to control the spin water and the injection amount of the release agent, and also the wettability and dryness of the aqueous release agent. And due to poor precision, the production cost increase due to the use of the release agent in a large amount is a problem.

따라서, 자동 분사 장치를 사용하여 이형제를 분사하는 경우 발생하는 분사량의 약 50%의 폐 이형제를 수집하여 흑연을 회수하여 재사용하고 있다. 구체적으로, 종래의 재활용 방법은 폐 이형제 용액을 운반하는 데 따른 운반비를 절감하기 위하여 황산 알루미늄(황산 반토)과 같은 응집제를 폐 흑연 이형제 용액에 투입하여 농축하여 운반하고 있으나, 응집제를 사용하더라도 흑연 함량을 약 15중량% 이상으로 농축하기 어려운 문제점을 가지고 있다. 한편, 흑연을 회수하기 위해서는 다량의 열을 가하여 용매를 증발시켜야 하므로 많은 에너지 비용이 소요되는 문제점을 가지고 있다.Accordingly, about 50% of the waste release agent is collected and the graphite is recovered and reused by injecting the release agent using the automatic injection device. Specifically, in the conventional recycling method, a coagulant such as aluminum sulfate (aluminum sulfate) is added to the waste graphite release agent solution in order to reduce the transportation cost associated with transporting the waste release agent solution. It is difficult to concentrate to about 15% by weight or more. On the other hand, in order to recover graphite, the solvent must be evaporated by applying a large amount of heat, which has a problem in that a large energy cost is required.

한편, 폐 흑연 이형제 용액을 재생하여 이형제로 다시 사용하고자 하는 시도도 있었으나, 재생 이형제 용액에서 악취가 나고 pH가 낮은 문제점은 차치하고, 상기에서 설명한 바와 같이 운반 비용을 절감하기 위하여 응집제를 사용하여 응집시킨 흑연이 다시 분산되지 않아서 이형제로서의 성능이 저하되는 문제점을 가지고 있었다.On the other hand, there have been attempts to regenerate the waste graphite release agent solution and use it again as a release agent. The graphite thus prepared was not dispersed again, so that the performance as a release agent was lowered.

따라서, 폐흑연 이형제 용액을 이형제 용액으로 효율적으로 재생할 수 있는 방법의 개발이 요구되어 왔다.Therefore, there has been a demand for the development of a method for efficiently recycling the waste graphite release agent solution into the release agent solution.

이에 본 발명은 수성 흑연 이형제 용액 금형에 자동 분사하는 경우 발생하는 다량의 폐 이형제 용액을 회수하여 재사용할 수 있도록 하는 수성 흑연 이형제 용액의 재생 방법을 제공하는 것을 목적으로 한다.Accordingly, an object of the present invention is to provide a method for regenerating an aqueous graphite release agent solution to recover and reuse a large amount of waste release agent solution generated when automatically spraying the aqueous graphite release agent solution mold.

본 발명의 목적에 따른 흑연 이형제 용액의 재생 방법은 TEA를 첨가하여 응집된 흑연을 재분산시키는 단계를 포함하여 구성된다.The method for regenerating the graphite release agent solution according to the object of the present invention comprises the step of adding TEA to redisperse the aggregated graphite.

첨가되는 TEA(triethylamine)의 양은 흑연 함량에 따라 적절히 가변될 수 있으며, 흑연 함량이 15~30중량%인 폐 흑연 이형제 용액에 대하여는 바람직하게 0.5~2.0중량%의 비율로 사용될 수 있다.The amount of added triethylamine (TEA) may be appropriately changed depending on the graphite content, and may be preferably used in a proportion of 0.5 to 2.0 wt% with respect to the waste graphite release agent solution having a graphite content of 15 to 30 wt%.

더욱 구체적으로, 본 발명의 흑연 이형제 용액의 재생 방법은 다음의 단계들을 포함하여 구성될 수 있다:More specifically, the method for regenerating the graphite release agent solution of the present invention may comprise the following steps:

a) 폐 흑연 이형제 용액에서 불순물을 제거하는 단계;a) removing impurities from the waste graphite release agent solution;

b) 폐 흑연 이형제 용액에 TEA를 첨가하여 응집된 흑연을 재분산시키는 단계;b) adding TEA to the waste graphite release agent solution to redisperse the aggregated graphite;

c) 임의로, 방부제를 첨가하는 단계.c) optionally, adding a preservative.

이하에서 본 발명을 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail.

통상적인 흑연 이형제 용액은 다음과 같이 제조된다.Conventional graphite release agent solutions are prepared as follows.

먼저, 90마이크론 메쉬를 90% 이상 통과하는 인상 흑연 또는 인조 흑연 분말을 분산제와 함께 물에 투입하여 분산시킨다.First, impression graphite or artificial graphite powder passing 90% or more through the 90 micron mesh is added to the water together with a dispersant to disperse it.

그 후, 안정제를 첨가한 후 1~2일동안 습식 분쇄하여 분산시킨다. 다음으로 바인더와 방부제, 소포제 등 첨가제를 첨가하여 제조한다. Thereafter, after the addition of the stabilizer, the product is wet-pulverized and dispersed for 1 to 2 days. Next, a binder, an antiseptic, an antifoaming agent, and the like are added to prepare the same.

최종 사용자는 위와 같이 제조된 흑연 함량 약 30중량%의 흑연 이형제 용액을 흑연 함량 약 2~3중량%로 물로 희석하여 사용한다.The end user may use the graphite release agent solution having a graphite content of about 30% by weight, diluted with water, with a graphite content of about 2-3% by weight.

희석된 흑연 이형제 용액을 금형에 자동 분사하면 약 50% 이상의 이형제 용액이 흘러 나오게 되며, 이는 폐기하거나 수집하여 재활용을 해야한다. 이 때, 위에서 설명한 바와 같이, 운반비를 절감하기 위하여 농축하여 부피를 줄여야 하는 바, 황산 알루미늄(황산 반토)를 이용하여 흑연을 응집시킨 후 침전시키고 상등액을 분리하여 약 15% 정도로 농축한다. Automatic injection of a diluted graphite release agent solution into the mold will cause more than about 50% release agent solution to flow out, which must be disposed of or collected and recycled. At this time, as described above, in order to reduce the transport cost should be concentrated to reduce the bar, the graphite is agglomerated and precipitated using aluminum sulfate (aluminum sulfate), and the supernatant is separated and concentrated to about 15%.

그런데 상기와 같이 농축된 이형제 용액을 재사용하는 데 있어서, 악취 및 낮은 pH 등 문제점 뿐만 아니라, 응집된 흑연 입자를 재분산시키기 어려운 문제점이 있다.However, in reusing the concentrated release agent solution as described above, there are problems such as odor and low pH, as well as difficult to redisperse the aggregated graphite particles.

본 발명은 이와 같이 흑연 응집체를 포함하는 이형제 농축액을 이형제로 재사용할 수 있도록 재생하는 방법에 관한 것이다.The present invention relates to a method for regenerating the release agent concentrate containing the graphite aggregate in such a way that it can be reused as the release agent.

본 발명의 흑연 이형제 용액 재생 방법은 먼저, 흑연 이형제 용액의 흑연 함량, 철분 함유 여부, pH 등을 분석한 후 적절한 물리적 처리를 통하여 불순물을 제거한다. 즉, 흡착포를 이용하여 기름 성분을 제거하고, 철분은 마그네틱 롤(magnetic roll)을 통과시켜 제거한다.The graphite release agent solution regeneration method of the present invention first analyzes the graphite content, iron content, pH, etc. of the graphite release agent solution, and then removes impurities through appropriate physical treatment. That is, the oil component is removed using an adsorption cloth, and iron is removed by passing through a magnetic roll.

그 후, TEA(tri ethyl amine)을 흑연 함량이 15~30중량%인 폐 흑연 이형제 용액에 대하여 0.5~2.0중량%의 비율로 투입하여 흑연 입자를 재분산시킨다. 황산 알루미늄을 사용하여 응집된 흑연 응집체는 물리적 방법으로는 재분산시키기가 어렵고, 황산 알루미늄으로 응집된 흑연 입자를 재분산시킬 수 있는 분산제도 지금까지는 알려지지 않았는데, 본 발명에서와 같이 TEA를 사용하면, 황산알루미늄에 의해 응집된 흑연이 잘 분산되는 효과가 발휘되는 것이다.Thereafter, triethyl amine (TEA) is added at a rate of 0.5 to 2.0% by weight relative to the waste graphite release agent solution having a graphite content of 15 to 30% by weight to redisperse the graphite particles. Graphite aggregates agglomerated using aluminum sulfate are difficult to redisperse by physical methods, and a dispersant capable of redispersing graphite particles agglomerated with aluminum sulfate is not known until now. The effect that the graphite aggregated by aluminum sulfate is well dispersed is exerted.

TEA를 투입하고 교반하여 재분산시킨 후 다시 흑연 함량, pH 기타 이형제로서의 물성을 체크한 후 필요시 방부제를 첨가하여 재생을 완료한다.After adding TEA, stirring and redispersing, check the graphite content, pH and other physical properties as a release agent, and if necessary, add a preservative to complete the regeneration.

이하에서 실시예를 통하여 본 발명을 상세히 설명한다. 그러나, 실시예는 본 발명이 속하는 분야에 종사하는 사람들에게 본 발명의 이해를 돕기 위하여 제공되는 것일 뿐 이에 의하여 본 발명이 한정되는 것은 아니며, 첨부하는 특허 청구의 범위에 의해서 본 발명의 보호 범위가 정해져야 한다.Hereinafter, the present invention will be described in detail through examples. However, the embodiments are provided only to help those of ordinary skill in the art to understand the present invention, and thus the present invention is not limited thereto. It must be decided.

실시예Example

흑연 함량이 20중량%이고 pH가 7.1인 폐 흑연 이형제 용액 1000kg을 흡착포를 이용하여 표면의 기름기를 제거한 후 TEA 16kg을 투입하고 1 시간동안 교반하여 흑연 입자를 재분산시켰다. 1000 kg of the graphite graphite releasing agent solution having a graphite content of 20% by weight and a pH of 7.1 was removed from the surface using an adsorption cloth, and 16 kg of TEA was added thereto, followed by stirring for 1 hour to redisperse the graphite particles.

재분산된 흑연 이형제의 pH는 알칼리성의 TEA에 의해 9로 상승하여 이형제로 사용하기에 적합한 pH가 되었다.The pH of the redispersed graphite release agent rose to 9 by alkaline TEA, making it a suitable pH for use as a release agent.

그 후 방부제로 SN315(제조사: 산노프코) 1 kg을 혼합하여 재생을 완료하였다.Thereafter, 1 kg of SN315 (manufactured by Sanofko) was mixed with a preservative to complete regeneration.

재분산된 흑연 이형제 용액을 30일 이상 동안 정치시켜 두었으나, 흑연 입자의 재응집은 관찰되지 않아서, 이형제로 재사용할 수 있음이 확인되었다.The redispersed graphite release agent solution was left to stand for 30 days or more, but no reagglomeration of the graphite particles was observed, and it was confirmed that it could be reused as a release agent.

본 발명에 의하여 수성 흑연 이형제 용액 금형에 자동 분사하는 경우 발생하는 다량의 폐 이형제 용액 중의 흑연을 효율적으로 재분산시킴으로서 이형제로 재사용할 수 있도록 하는 수성 흑연 이형제의 재생 방법이 제공된다.The present invention provides a method for regenerating an aqueous graphite release agent which can be reused as a release agent by efficiently redispersing graphite in a large amount of waste release agent solution generated when automatically spraying into an aqueous graphite release agent solution mold.

Claims (5)

TEA(triethylamine)를 첨가하여 응집된 흑연을 재분산시키는 단계를 포함하는 폐 흑연 이형제 용액의 재생 방법.Re-dispersing the aggregated graphite by the addition of triethylamine (TEA). 제1항에 있어서, TEA는 흑연 함량이 15~30중량%인 폐 흑연 이형제 용액에 대하여 0.5~2.0중량%의 비율로 사용되는 것을 특징으로 하는 폐 흑연 이형제 용액의 재생 방법.The method for regenerating the waste graphite release agent solution according to claim 1, wherein TEA is used at a ratio of 0.5 to 2.0 wt% based on the waste graphite release agent solution having a graphite content of 15 to 30 wt%. a) 폐 흑연 이형제 용액에서 불순물을 제거하는 단계;a) removing impurities from the waste graphite release agent solution; b) 폐 흑연 이형제 용액에 TEA를 첨가하여 응집된 흑연을 재분산시키는 단계;를 포함하는 폐 흑연 이형제 용액의 재생 방법.b) re-dispersing the aggregated graphite by adding TEA to the waste graphite release agent solution. 제3항에 있어서, The method of claim 3, c) 방부제를 첨가하는 단계를 추가로 포함하는 폐 흑연 이형제 용액의 재생 방법.c) A method of regenerating a waste graphite release agent solution further comprising adding a preservative. 제3항 또는 제4항에 있어서, TEA는 흑연 함량이 15~30중량%인 폐 흑연 이형제 용액에 대하여 0.5~2.0중량%의 비율로 사용되는 것을 특징으로 하는 폐 흑연 이형제 용액의 재생 방법.The method for regenerating the waste graphite release agent solution according to claim 3 or 4, wherein the TEA is used at a ratio of 0.5 to 2.0% by weight relative to the waste graphite release agent solution having a graphite content of 15 to 30% by weight.
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KR20180052972A (en) * 2016-11-11 2018-05-21 주식회사 카보랩 Reproducing Method of Waste carbon powder and carbon block manufacturing thereof

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JPS61235036A (en) 1985-04-10 1986-10-20 Toyota Motor Corp Chemical composition for regeneration of graphite lubricating release agent
KR970015687A (en) * 1995-09-25 1997-04-28 오세근 Paste Aqueous Coating Composition
KR20010049932A (en) * 1999-07-30 2001-06-15 빌프리더 하이더 Coating Compositions
JP2006159208A (en) 2004-12-02 2006-06-22 Masanao Matsui Release agent reproducing system and method for measuring graphite concentration in release agent

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JPS61235036A (en) 1985-04-10 1986-10-20 Toyota Motor Corp Chemical composition for regeneration of graphite lubricating release agent
KR970015687A (en) * 1995-09-25 1997-04-28 오세근 Paste Aqueous Coating Composition
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20180052972A (en) * 2016-11-11 2018-05-21 주식회사 카보랩 Reproducing Method of Waste carbon powder and carbon block manufacturing thereof
KR101963812B1 (en) * 2016-11-11 2019-03-29 주식회사 카보랩 Reproducing Method of Waste carbon powder and carbon block manufacturing thereof

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