R&D Reports

FY 1998

vol. 1998 - II (1998.11.30 issue)

In order to remove highly harmful impurity such as arsenic from drinking water, co-precipitation method is usually used in large scale water treatment plants.
But recently some simple and compact adsorbing processes have been adopted in small scale plants using activated alumina et al.
In this article newly developed arsenic removing and remaking processes by activated alumina are described together with an outline of co-precipitation method.
( by Kazuo HORINOUCHI, Toshio ASHITANI )

With the recent spectacular development of science and technology, the volume of information treated by human society has increased vastly. In this way, our today's information-intensive society is heavily dependent on the personal computer (PC) system, which deftly handles the blooding flux of information in the area of business and private life. Recently, a liquid crystal display (LCD), especially a color TFT-LCD is used widely as a display system for PC.
In this paper, we review the production methods and the features of a color filter which is one of the most important parts for color LCD's. Among the several production methods for color filters, we emphasize into the pigment disperse type color filters which are prevailing widely in various a pplications.
( by Hiromu KORI, Nobuya NII ZAKI, Toshihisa DEGUCHI, Yukio FUJII )

We investigated conditions of in vitro propagation of garlic cultivar 'Howaito-roppen' and established a production system of high-quality seed bulbs of garlic, which consists of meristem-tip culture, in vitro propagation of bulblets, cultivation of the bulblets in an insect-proof house, and selecting elite clones. The obtained conditions are as follows; (1) meristem-tips are cultured on LS medium with 1??M IAA + 1??M BA, (2) shoots are propagated on modified LS medium (56.5 mM KNO3 and 3.5 mM NH4Cl) with 5??M NAA and 10??M BA, (3) shoots are cold-treated at 5 degree C for 4 to 6 months, then cultured on LS medium with 9% sucrose for bulbing. Bulblets are planted into trays to grow nurseries, then transplanted into the insect-proof house. Bulbs with cloves were obtained with high efficiency through one year cultivation of bulblets. The garlic seed bulbs were cultivated in farmer's open fields, and re-infection of viruses was rarely found in an isolated field. High quality seed bulbs obtained through the production system showed 1.5 to 1.9 times higher yield compared to that of the common garlic.
( by Takayuki NAGAKUBO, Miyuki TAKAICHI, Kenji OEDA, Satoru NAGATA )

COLOR JUDGE is the Automated Spectro-Photometric Control System instrumental in controlling delicate hues and shades of colored products in process, where product color and its control is of vital importance. In many industrial process, visual inspection of products by experienced operators at final stage has been critical and it often has been found restrictive in raising overall production performance. COLOR JUDGE consists of advanced units and devices as well as the software of the latest version, and consequently offers sensitiveness comparable to visual inspection and assures constant and continued reliability.
Uniqueness of COLOR JUDGE lies in employing a spectro-photometer which has been developed and fabricated by MINOLTA specifically for the purpose of creating the system applicable to precise color control in various production lines. The high-sensitive spectro-photometer promises a great advantage of COLOR JUDGE over many other color judge systems which commonly use CCD camera as a sensor. Besides, color correction function, which is not feasible with most of existing systems has been added to the upgraded software of COLOR JUDGE.
( by Yuzuru TAKAHASHI, Takahisa SHINKAWA, Michinari NAKASE, Naoki KATO )

Under-coating and its effect on the printability of double-coated paper were studied. Five under-coated papers which were designed to have different coating structures were prepared and coated with same top-color. The printabilities such as inkset and printgloss of these double-coated papers were evaluated. The structures of under-coatings were analyzed and relation between the structure of under-coating and the printability of double-coated paper was discussed.
( by Yoshihiko HATTORI, Kenichi YAMAZAKI )

2,4-Dichloro-3-ethyl-6-nitrophenol (DCENP) is key intermediate for cyancoupler of photographic paper.
We developed and industrialized the new and more rational DCENP production process based on aqueous system.
( by Yasuhiko HORIKAWA, Masaya YAMASHITA, Kazutaka MORINO, Shin-ichi KOYAMA, Mitsuhiro WADA, Seiji MAKI )

Recent development of molecular genetics and transgenic technologies have provided us with the capability to selectively add or delete defined genes into living animals.
Transgenic animal models should advance toxicology, regulatory science and public health by applying more relevant methods for evaluating human risk.
Applications for transgenic mice in the field of mutagenicity and carcinogenicity studies are reviewed herein.
( by Satoshi UWAGAWA, Keisuke OZAKI, Toru YAMADA, Tokuo SUKATA )

Recently, due to the high performance of computer and developments of software, simulations with theoretical chemical methods become familiar to experimental chemists. This review describes a few examples of our theoretical approach on catalyst design for olefin polymerization. We introduced more realistic models and revealed the role of not only the substituents of ligands but also last inserted monomer for the detailed analysis of metallocene catalyst system and succeeded to get more precise information of insertion reaction. In near future, collaboration of experimental chemists and theo-retical chemists might lead the development of highly efficient catalyst.
( by Hiroshi KURIBAYASHI, Tatsuya MIYATAKE )

Defect control in manufacturing process for semiconductor is becoming more important as the scale of integration increase. SURFSCAN, OM, SEM and KLA are used for convenient tools of defect control. Recently many semiconductor makers adopt the defect inspection system of the KLA company which can rapidly and precisely detect the variety of defect on the wafer to increase the yield of their product.
We introduced KLA-2132 to improve our products and user supports.
Here we described the advantage of the defect inspection tool of KLA system, and the application of KLA-2132 to inspect the defect originated in lithography process, and materials for photoresist.
( by Yukio HANAMOTO, Takayuki MIYAGAWA, Yukoh TAKAHASHI )

In chemical plants, polymers play an important role as resistive materials in aggressive corrosion environments. When degradation of materials causes equipment to break down, it is very important to investigate the degradation mechanisms in order to take suit able countermeasures to prevent similar occurrences. The accumulated knowledge from such investigations will help increase the safety and reliability of the polymers used as plant materials.
This article describes investigations of the degradation of polymers used in chemical plant equipment.
( by Mikitoshi NAKADA )

vol. 1998 - I (1998.5.25 issue)

A new synthetic pyrethroid imiprothrin (Pralle® T) with super knockdown activity has been developed for household use. The knockdown activity against cockroaches was much superior to that of conventional pyrethroids such as tetramethrin ( Neo-pynamin® ) and prallethrin ( Etoc® ).
Almost all physical and chemical properties of Pralle® T were suitable for the formulations of household insecticides except for its high viscosity. In order to make easy for handling, Pralle® T was dissolved in isopropyl myristate to make the manufacturing use product (MUP), named as Pralle®. Pralle® can be widely used as a super knockdown agent for household use. Pralle® was actually formulated as an aerosol (Pralle® C) for cockroach control. Moreover, the mixture with killing agent such as Gokilaht® is also recommendable for its practical application.
In this article, characteristics of Pralle® T,Pralle® (MUP) and Pralle® C (aerosol) are described about various aspects such as screening, chemistry, physical and chemical properties, formulation, performance and toxicology.
( by Masachika HIRANO, Tadahiro MATSUNAGA, Hideo KANEKO, Ritsuko FURUTA, Shigeki YOKOI )

Poly Methyl Methacrylate (PMMA) is widely used as transparent material. But because of its low scratch resistance,hard coating process is occasionally treat ed. Recently, it is required not only surface hardness but anti-static property to keep off dusts and stain. We have investigated the addition of anti-static property to hard coated layer, therefore we have developed acrylic sheets that has both hardness and anti-static property.
In this report, Anti-static hard coating process is summarized.
( by Yukio YASUNORI, Shinsuke OCHIAI, Yoshimi NAKAGAWA, Tsutomu YAMAMOTO )

Pyridine bases are widely used in pharmaceuticals, insecticides, and herbicides due to their high bioactivity. In this paper, some typical synthetic methods for pyridine bases, recent advances of catalysts having a shape selectivity of pentasil zeolite (ZSM-5) with a similar pore diameter to pyridine ring, and some considerations on their catalysis are described.
( by Nobuyuki ABE )

Since the discovery of highly active homogeneous catalyst systems based on metallocene and methylalumoxane,many studies have been made from the point of view of both scientific interest and industrial use. This review describes mainly a recent progress in the studies of olefin polymerization with metallocene catalyst systems and stereoregulation mechanisms of the propylene polymerization. Novel non-metallocene catalysts and new polymer synthesis with such catalysts are also described.
( by Tatsuya MIYATAKE, Akio IMAI )

Needs for aromatic sulfur compounds are increasing for use in highly functional materials such as pharmaceuticals, agricultural chemicals, materials with high-refractive index, anti-oxidants and the like.
On the other hand, concerning the synthetic techniques of the aromatic sulfur compounds, conventional methods have been lacking in general-purpose use, because each compound was manufactured by a specific method different from the others.
The present technique relates to the development of new widely-used synthetic methods of high-functional aromatic sulfur compounds basically comprising two processes of "Introduction of thioalkyl group and cleavage of thio-alkyl bond", using an alkylmercaptan as a sulfur source.
( by Hiroshi GODA, Hirokazu KAGANO )

We restructured a data-processing-system for animal toxicity studies in which main frame computer worked as a host machine into a new system in which personal computers of the client/the server types are playing the leading role of the system. The new system outperforms the old system in terms of the data processings as well as the flexibility for the revision of the softwares.
The new system comprises seven PC-servers (NEC Express 5800 series) with WindowsNT3.51 and data base system of Oracle 7.2,and 75 PC-cliants (NEC PC98 series) with Windows95. The network is operated by Oracle SQL*Net.
Details of the restructuring and characteristic and performance of the new system, New-TOPS21 (New-TOxicity data total Processing System 21), are described.
( by Yasuo MATSUMOTO, Naohiko ISOBE, Hajime KAWASAKI )

It is revealed that concentration level of airborne molecular contaminants such as organic compounds is by far higher in than that of particle in cleanroom air. The airborne molecular contaminants become an increasing serious problem because of further integration of semiconductor device. Especially, several kinds of organic compounds, including phthalates, phosphates and siloxanes, strongly affect device performance.
This article describes the origin of molecular contaminants, the influence in electronic device performance, the analytical methods of cleanroom air, the adhesive mechanism onto silicon wafer surface, and techniques for preventing molecular contaminants.
( by Taketoshi FUJMOTO, Kikuo TAKEDA )

By using newly developed matrix-assisted laser desorption/ionization (MALDI) technique combined with time-of-flight mass spectrometry (TOFMS), we have been able to obtain mass spectra of various kinds of synthetic polymers of molecular weight above 10k Da. It has the potential to characterize polymers and oligomers with great accuracy and precision for molecular weight and end group determination.
This paper illustrates the principle and the features of MALDI-TOFMS, measurement techniques for obtaining a high quality mass spectrum, and also some applications of polymeric materials for fine chemicals.
( by Stoshi ASANO, Kiyoshi YAMAMOTO, Osamu HIROAKI, Mitsumori KATOH )

This paper provides purposes of pesticide formulations and recent requirements of pesticide industry in the first place. Kind of formulations and trend of their manufacturing amounts are shown. Then problems of conventional formulations, their improvement methods and resulting new formulations are explained.
New promising formulations such as water-based formulations, water dispersible granules, jumbo herbicides, 1 kg granules, water surface spreading formulations, microcapsules, fertilizer containing pesticides and physical controlling methods are reviewed, where their advantages and trends are also discussed.
( by Kozo TSUJI )

Molecular structure of PPE-PA linkage part of PPE-PA alloy, which is thought to be very important for stabilizing PPE and PA boundary in PPE-PA alloy, was determined by the use of high field nuclear magnetic resonance (NMR). Methods for NMR sample preparation and technique to obtain high quality two-dimensional (2D) NMR spectra were established. NMR sample preparation was performed in 2 steps: (1) isolation of PPE-PA block copolymer by extracting PPE and PA which do not react, and (2) mild acid treatment which cleaves only amide bond of PA but not imide bond. Two types of PPE-PA linkage structure were determined by analyzing 2D-NMR spectra (HMQC,HMBC and TOCSY) and confirmed by 13C labeling study. These structures indicated that acid anhydride moiety of compatibilizer delivative formed imide bond with NH2 end group of PA and that its unsaturated bond reacted with PPE to yield PPE-PA block copolymer.
( by Ryozo ISHIMOTO, Takashi KATO )

Remarkable increase of both the catalytic activities and the selectivities of t he desired products (selectivity of dimers based on the reacted propylene, selectivity in C6 olefins) has been attained for dimerization of propylene by nickel-phosphine catalyst systems especially in the presence of strong sulfonic acid (such as MeSO3H, CF3SO3H) and/or dialkyl sulfate (such as Me2SO4, Et2SO4). It turned out that the product distribution in dimers is highly dependent upon the steric factor of tert-phosphine ligand used: the electronic nature of tert-phosphine plays a role for the high activity. 31P-NMR spectrum of the catalyst solution showed a peak at 33 ppm (JP-H=458 Hz): the corresponding peak on 1H-NMR was observed at 4.3 ppm which could be confirmed by 2D NMR (31P-1H, COSY) and 1H-NMR with 31P (33 ppm) selective decoupling. The 27Al-NMR spectrum of the same solution showed a relatively sharp resonance at 60 ppm.
( by Kotohiro NOMURA, Gohfu SUZUKAMO, Michiko YAMAMOTO, Makoto ITAGAKI )