KR960012217B1 - Process for the production of high colouring carbon black - Google Patents
Process for the production of high colouring carbon black Download PDFInfo
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- KR960012217B1 KR960012217B1 KR1019930016434A KR930016434A KR960012217B1 KR 960012217 B1 KR960012217 B1 KR 960012217B1 KR 1019930016434 A KR1019930016434 A KR 1019930016434A KR 930016434 A KR930016434 A KR 930016434A KR 960012217 B1 KR960012217 B1 KR 960012217B1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2405—Stationary reactors without moving elements inside provoking a turbulent flow of the reactants, such as in cyclones, or having a high Reynolds-number
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/245—Stationary reactors without moving elements inside placed in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00159—Controlling the temperature controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
Abstract
Description
제1도는 본 발명의 실시예에 이용된 장치를 나타낸 단면도.1 is a cross-sectional view showing a device used in an embodiment of the present invention.
* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : 연소실 2 : 연소오일 도입관1: combustion chamber 2: combustion oil introduction pipe
3 : 연소공기 도입구 4 : 트로트부위3: Combustion air inlet 4: Trot part
5 : 반응실 6 : 원료오일 도입관5: reaction chamber 6: raw material oil introduction pipe
7 : 급냉수 도입관7: quenching water introduction pipe
본 발명은 흑색안료로 사용되는 고착색력 카본블랙의 제조방법에 관한 것으로, 다시 말하면 플라스틱, 페인트 또는 잉크중에 분산될 경우 착색력이 우수한 카본블랙에 관한 것이다.The present invention relates to a method for producing a high coloring power carbon black used as a black pigment, that is, to a carbon black having excellent coloring power when dispersed in plastic, paint or ink.
훠니스 카본블랙(furnace carbon black)은 일반적으로 반응로내의 열기류 중에 도입된 원료오일이 1,000 내지 1,500℃정도의 고온 분위기에서 탈수소반응을 수반하는 중합을 반복하여 결정자가 형성되고 이 결정자가 다수 응집하여 카본블랙 입자로 되는 과정을 거쳐 생산된다. 이 입자 형성기의 카본블랙은 용융상태 또는 이와 유사한 상태로 입자 상호간의 충돌에 의해 화학적 결합 또는 물리적 응집력 등에 의해 연쇄상 구조를 만드는 것으로 알려져 있다. 따라서 훠니스법에 의해 생성되는 카본블랙의 물성은 반응로의 형태, 열기류체의 온도 및 유체 역학적인 상태, 원료오일의 도입량, 도입 노즐, 반응온도, 반응시간 등에 의해 변화한다. 통상 카본 블랙은 입자크기가 작을수록 구조의 발달정도가 낮을수록 착색력이 향상되는 경향이 있다.Furnace carbon black is generally formed by crystallization by repeating polymerization involving dehydrogenation in a high-temperature atmosphere of 1,000 to 1,500 ° C. Produced through a process of forming carbon black particles. Carbon black of this particle forming machine is known to form a chain-like structure by chemical bonding or physical cohesion by collision between particles in a molten state or similar state. Therefore, the physical properties of the carbon black produced by the varnish method vary depending on the shape of the reactor, the temperature and hydrodynamic state of the hot air body, the amount of raw material oil introduced, the introduction nozzle, the reaction temperature, the reaction time, and the like. In general, carbon black has a tendency that the smaller the particle size, the lower the degree of development of the structure, the coloring power is improved.
안료의 착색력은 어떤 안료가 특정의 보조안료의 일정량을 착색하는 능력을 말한다. 흑색안료로 사용되는 카본블랙의 경우, 백색안료와 섞었을 때 이것을 검게 하는 능력을 말한다.The coloring power of a pigment refers to the ability of a pigment to color a certain amount of a particular auxiliary pigment. In the case of carbon black used as a black pigment, it refers to the ability to blacken it when mixed with a white pigment.
일반적으로 질소흡착(BET) 비표면적이 (N2SA)이 230m2/g이상, 다시말하면 평균 입자경 16nm이하의 카본블랙 즉, 입자가 매우 작아서 고착색력을 가지는 카본블랙은 표면적이 크므로 플라스틱이나 페인트 또는 잉크중에 분산될 경우 입자 크기가 큰 카본블랙보다 분산에 많은 에너지를 필요로 하므로 상대적으로 분산이 어렵다. 분산이 곤란하게 되면 카본블랙의 입자크기가 작아짐에 따른 착색력 증가효과를 상쇄하게 된다.In general, the specific surface area (N 2 SA) of nitrogen adsorption (BET) is 230 m 2 / g or more, that is, carbon black having an average particle diameter of 16 nm or less, that is, carbon black having high coloration ability because the particles are very small, When dispersed in paints or inks, dispersion is relatively difficult because more energy is required for dispersion than carbon black having a large particle size. If it is difficult to disperse, the effect of increasing the coloring power as the particle size of the carbon black becomes smaller is cancelled.
본 발명은 상기 문제점을 해소하고 질소흡착(BET) 비표면적(N2SA) 200m2/g,다시 말하면 평균 입자경 18nm 전후의 입자경 영역에 있으며, 플라스틱, 페인트 또는 잉크중에 분산될 경우 착색력이 우수한 카본블랙을 제공함을 목적으로 한다.The present invention solves the above problems and the nitrogen adsorption (BET) specific surface area (N 2 SA) 200m 2 / g, that is, in the particle size region around 18nm average particle diameter, and excellent in colorability when dispersed in plastic, paint or ink The purpose is to provide black.
본 발명은 질소흡착(BET) 비표면적(N2SA)이 190 내지 210m2/g, 디부틸 프탈레이트 흡수값(Dibutyl phthalate absorption number) 50 내지 70ml/100g을 가지며 질소흡착(BET) 비표면적(N2SA)과 요오드 흡착량(Iodine adsorption number)의 차가 8.5-10.5의 특성요건을 만족하는 카본블랙에 의해 달성된다.The present invention has a nitrogen adsorption (BET) specific surface area (N 2 SA) of 190 to 210m 2 / g, Dibutyl phthalate absorption number of 50 to 70ml / 100g and a nitrogen adsorption (BET) specific surface area (N The difference between 2 SA) and the iodine adsorption number is achieved by carbon black satisfying the characteristic requirements of 8.5-10.5.
본 발명의 카본블랙은 동일한 비표면적의 레벨에서 착색력이 현저히 높은 특성을 나타낸다.The carbon black of the present invention exhibits a property of remarkably high coloring power at the same specific surface area level.
본 발명의 특성을 가지는 카본블랙은 카본블랙 제조용 반응로내에서 연소공기와 연료오일을 연소시켜 생성된 열기류체에 원료오일을 반응로내에 공급하여 열분해시켜 카본블랙으로 전환시키고, 반응 중지수를 가해 급냉시키는 단계를 포함하는 훠니스 카본블랙의 제조방법에서, 반응로내의 반응조건과 생성 카본블랙의 반응로내 체류시간을 제어함에 의해 얻을 수가 있다.The carbon black having the characteristics of the present invention is converted into carbon black by supplying the raw material oil into the reaction furnace and thermally decomposing the carbon dioxide produced by combusting combustion air and fuel oil in the reactor for producing carbon black, and converting the reaction into carbon black. In the method for producing a wellness carbon black comprising a step of quenching, it can be obtained by controlling the reaction conditions in the reactor and the residence time of the produced carbon black in the reactor.
본 발명에 관한 카본블랙은 통상적인 방법에 따라 플라스틱, 페인트 또는 잉크에 배합된다. 질소흡착(BET) 비표면적(N2SA)이 190 내지 210m2/g으로 종래 품종의 고착색력 카본블랙이나 작음으로 기인하는 착색력의 낮음을 질소흡착(BET) 비표면적(N2SA)과 요오드 흡착량의 차를 종래 품종의 카본블랙보다 낮은 8.5 내지 10.5로 조정함에 의해 효과적으로 향상할 수 있다.Carbon black according to the present invention is blended into plastics, paints or inks according to conventional methods. Nitrogen adsorption (BET) specific surface area (N 2 SA) is 190 to 210 m 2 / g, the low coloration power due to the high colorability carbon black or small size of conventional varieties BET specific surface area (N 2 SA) and iodine By adjusting the difference of the adsorption amount to 8.5 to 10.5, which is lower than that of the conventional carbon black, it can be effectively improved.
이하, 도면의 의거 본 발명을 설명하기로 한다.Hereinafter, the present invention will be described based on the drawings.
본 발명의 카본블랙은 첨부된 도면과 같은 장치에 의해 준비되었다. 제1의 1은 원통상의 내부공간을 가지는 연소실이다. 입구 내경 800mm, 출구 내경 400mm길이 2800mm의 연소실(1)에는 연소오일 도입관(2)과 연소공기 도입구(3)가 장치되어 있다. 그리고 이 연소실(1)에는 이것과 동축방향으로 내경 300mm의 트로트 부위(4)를 통하여 내경 500mm 길이 1200mm의 반응실(5)이 연결되어 있으며, 트로트 부위(4)에는 종방향으로 원료오일을 도입하기 위한 원료오일 도입관(6)이 설치되어 있고 이 도입관(6)에는 분사노즐(6,)이 장치되어 있다. 반응실(5)에는 반응을 중지시키는 급냉수를 분사하기 위한 급냉수 도입관(7)이 설치되어 있다.Carbon black of the present invention was prepared by the apparatus as shown in the accompanying drawings. The first 1 is a combustion chamber having a cylindrical inner space. The combustion oil inlet pipe 2 and the combustion air inlet port 3 are provided in the combustion chamber 1 having an inlet diameter of 800 mm and an outlet diameter of 400 mm and a length of 2800 mm. The combustion chamber 1 is connected to a reaction chamber 5 having an inner diameter of 500 mm and a length of 1200 mm through a trot portion 4 having an inner diameter of 300 mm in the coaxial direction thereof, and a raw material oil is introduced into the trot portion 4 in the longitudinal direction. The raw material oil introduction pipe 6 for this purpose is provided, and the injection pipe 6 is equipped with the injection nozzles 6 and it. The reaction chamber 5 is provided with a quench water introduction pipe 7 for injecting quench water to stop the reaction.
이상과 같이 구성된 본 발명은 연소실(1)에 카본블랙 상에 생성에 필요한 반응열을 충분히 공급하기 위하여 연소오일 도입관(2)과 연소공기도입이구(3)를 통해 연소오일과 연소공기가 도입된다.In the present invention configured as described above, the combustion oil and the combustion air are introduced through the combustion oil introduction pipe 2 and the combustion air inlet 3 so as to sufficiently supply the reaction heat necessary for generation on the carbon black to the combustion chamber 1. .
연소실(1)내에서의 연소오일과 연소공기의 연소에 의하여 생성된 고온연소가스를 트로트(4)를 통하여 연결된 반응실(5)로 이동하게 되며, 이때 트로트(4)에 설치된 원료오입관(6)을 통하여 원료오일을 분무한다.The high temperature combustion gas generated by combustion oil and combustion air in the combustion chamber 1 is moved to the reaction chamber 5 connected through the trot 4, and at this time, a raw material inlet pipe installed in the trot 4 ( Spray raw material oil through 6).
이렇게 분무된 원료유는 반응실(5)에서 일부는 연소되고 일부는 열분해가 진행되어 탈수소화, 핵화, 고분자화 카본블랙입자형성, 구조발달 및 응집체 형성등의 과정을 거쳐 카본블랙을 생성하게 된다. 생성된 카본블랙을 함유한 고온가스는 반응실(5)에서 카본블랙 포집공정으로 이동하면서 급냉수 도입관(7)을 통하여 분사되는 급냉수에 의하여 급냉이 이루어지며 카본블랙 생성반응이 종결되게 된다.The crude oil sprayed in this way is partially burned in the reaction chamber 5, and partly pyrolyzed to produce carbon black through dehydrogenation, nucleation, polymerized carbon black particle formation, structure development and aggregate formation. . The hot gas containing the produced carbon black is quenched by the quench water sprayed through the quench water introduction pipe 7 while moving from the reaction chamber 5 to the carbon black collection process, and the carbon black formation reaction is terminated. .
이하, 본 발명을 실시예에 의해 보다 구체적으로 설명한다.Hereinafter, an Example demonstrates this invention more concretely.
본 발명에 사용된 원료오일을 아래와 같은 성분의 석탄계 크레오소오트유와 석유계의 플로다이지드 카탈리스틱 크래이킹 바텀유(FCC)이다.The raw material oils used in the present invention are coal-based creosote oils and petroleum-flooded catalytic cracking bottom oils (FCC) having the following components.
본 발명에 사용된 원료 오일Raw oil used in the present invention
[표 1]TABLE 1
실시예에서 제조되는 카본블랙의 물성을 평가하는데 사용되는 시험법은 다음과 같다.The test method used to evaluate the physical properties of the carbon black produced in the Example is as follows.
1. N2SA : ASTM D3037에 의한 방법에 따라 카본블랙 입자표면에 질소를 흡착시켜 흡착된 질소의 양을 측정함으로써 카본블랙입자 표면적을 측정한다.1. N 2 SA: Carbon black particle surface area is measured by adsorbing nitrogen on the surface of carbon black particles according to the method according to ASTM D3037 and measuring the amount of adsorbed nitrogen.
2. 요오드 흡착량 : ASTM D1510의 방법에 따라 카본블랙입자 표면에 Iodine을 흡착시켜 단위 g당 흡착된 Iodine의 량(mg)을 측정하므로써 카본블랙의 입자 표면적을 측정한다.2. Iodine adsorption amount: The particle surface area of carbon black is measured by measuring the amount (mg) of adsorbed iodine per gram by adsorbing iodine on the surface of carbon black particles according to the method of ASTM D1510.
3. DBP흡유량 : ASTM D2414에 의한 방법에 따라 카본블랙 입자표면에 디부틸 프탈레이트 용액을 흡수시켜 흡수된 양을 측정하므로써 카본블랙 입자의 구조발달 정도를 측정한다.3. DBP oil absorption: The degree of structural development of carbon black particles is measured by absorbing dibutyl phthalate solution on the surface of carbon black particles according to the method according to ASTM D2414.
4. pH치 : ASTM D1512에 의한 방법에 따라 일정량의 시료를 분쇄하여 증류수와 함께 끓여서 상등액을 버린 후 그 술러지의 pH를 pH미터로 측정한다.4. pH value: According to the method according to ASTM D1512, a predetermined amount of the sample is ground, boiled with distilled water, discarded the supernatant, and then the pH of the sagage is measured with a pH meter.
5. 휘발성 물질 : 일정량의 시료를 일정온도(950℃)로 유지되는 전기로 내에 7분간 방치한 후 냉각시켜 시료의 감량을 측정하므로써 휘발성 물질의 함량을 측정한다.5. Volatile substances: A certain amount of sample is placed in an electric furnace maintained at a constant temperature (950 ℃) for 7 minutes and then cooled to measure the weight loss of the sample.
6. 체잔분(#325) : 카본블랙을 1.7 내지 2kg/cm2의 고수압 물로 세척하고 남은 체잔분의 양을 측정하는 것으로 체잔분의 주요 성분들을 내화물, 철분, 볼코크 등이다.6. Body residue (# 325): Wash carbon black with 1.7 ~ 2kg / cm 2 high-pressure water and measure the amount of residual body residue. The main components of body residue are refractory, iron and ball coke.
7. 착색력 : 카본블랙을 백색안료와 같이 비히클에 섞어 페이스트상으로 만든 다음 유리판에 도포하였을때의 색의 밝기를 나타내는 것으로 색이 짙을수록 착색력이 강한 것을 의미한다. ASTM D3265에 의한 방법에 따라 카본블랙 시료와 산화아연 및 아마인유를 후버 타이프멀러(Hoover type muller)로 혼합하여 페이스트(Paste)로 만든 다음, 유리판위에 필름어플리케이터(Film applicator)를 사용하여 정해진 두께의 필름으로 만든다. 다음에 반사광도계(densichron reflectronmeter)를 사용하여 시료의 측정값과 표준 카본블랙시료(IRB #3)의 측정값을 대비하여 상대적인 수치로서 나타낸다. 카본블랙 시료의 착색력은 다음의 식에 의해 산출된다.7. Coloring power: Carbon black is mixed with vehicle like white pigment to make paste, and it shows the brightness of color when applied to glass plate. The darker the color, the stronger the coloring power. According to the method according to ASTM D3265, carbon black sample, zinc oxide and linseed oil are mixed with Hoover type muller to make a paste, and then a film applicator is used on a glass plate to have a predetermined thickness. Made of film Next, the measured value of the sample is compared with the measured value of the standard carbon black sample (IRB # 3) using a densitometric reflectronmeter, and is shown as a relative numerical value. The coloring power of a carbon black sample is computed by the following formula.
T=×100T = × 100
T : 시료의 착색력T: coloring power of sample
S : 시료의 측정값S: measured value of the sample
I : 표준 카본블랙의 측정값I: measured value of standard carbon black
실시예 1 내지 5Examples 1-5
실시예 1 내지 5에서 제조한 카본블랙의 물성은 표 2와 같다. 또한, 비교예 1 내지 3에서 시판되고 있는 안료용 카본블랙의 물성은 표 2와 같다.Physical properties of the carbon black prepared in Examples 1 to 5 are shown in Table 2. In addition, the physical properties of the carbon black for pigments commercially available in Comparative Examples 1 to 3 are shown in Table 2.
본 발명에 사용된 원료오일Raw material oil used in the present invention
[표 1]TABLE 1
상기 표 2로부터 실시예 1 내지 5에 의해 제조된 카본블랙은 종래의 기술에 의해 제조된 동일 입자크기의 카본블랙에 비해 착색력이 크게 증가하였음을 알 수 있다. 또 BET 비표면적(N2SA)이 230m2/g을 넘는 카본블랙에 대하여도 착색력이 손색없음을 알 수 있다.It can be seen from the above Table 2 that the carbon black prepared in Examples 1 to 5 significantly increased the coloring power compared to the carbon black having the same particle size manufactured by the prior art. In addition the BET specific surface area (N 2 SA) of carbon black is even for more than 230m 2 / g It can be seen that no color strength is inferior.
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| KR100755415B1 (en) * | 2005-12-30 | 2007-09-04 | (주)디피아이 홀딩스 | Cationic electrodeposition coating composition and method of preparing the same |
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